Sep-21 News Extracurricular laboratory: Synthetic route of 13070-45-6

According to the analysis of related databases, 13070-45-6, the application of this compound in the production field has become more and more popular.

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 13070-45-6 as follows. HPLC of Formula: C13H15NO

Dissolve 93 mg of S11 in acetonitrile.Add 135 mg of 3,4-dihydroxybenzonitrile and add 7 mg of iron phthalocyanine under ice bath.30 mg of acetic acid, 4.8 mg of methanesulfonic acid and 135 mg of tert-butyl hydroperoxide, After stirring the reaction for 5 minutes under the same conditions,After monitoring the reaction, it was diluted with 20 mL of ethyl acetate and extracted with 20 mL of H2O.The combined organic layer Wash with 20 mL of saturated brine.Dry with anhydrous Na2SO4, filter and spin dry. Purified with silica gel column, eluent PE/ EtOAc = 8:1,188 mg of compound 11,The reaction yield was 56%;The product was a light yellow oil at room temperature.Physical state: light yellow oil; melting point: 138.5-139.4 C

According to the analysis of related databases, 13070-45-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Fuzhou University; Chen Haijun; Guo Mei; Ye Jinxiang; Chen Yi; Lin Yuqi; Gao Yu; (14 pag.)CN108530456; (2018); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Some tips on 6-Methoxy-1,2,3,4-tetrahydrocarbazole

The synthetic route of 13070-45-6 has been constantly updated, and we look forward to future research findings.

Related Products of 13070-45-6, A common heterocyclic compound, 13070-45-6, name is 6-Methoxy-1,2,3,4-tetrahydrocarbazole, molecular formula is C13H15NO, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

General procedure: A stirred solution of acrylate 9 (1 mmol), cycloalkaneindole 10a,b, 11a-j, 12a,b, or 13a,b, (1 mmol), CsF (0.1 g), and hydroquinone (0.02 g) in DMF (1.5 mL) was heated at 120-140C for 4 h. The solvent was removed in vacuo (3 Torr), the residue was extracted with dichloromethane, the solvent was removed in vacuo. Column chromatography of the residue (silica gel (60 mesh), elution with methanol-chloroform, 1 : 10) afforded target compounds. This procedure was applied for the synthesis of the following compounds: 1-[3,7-bis(dimethylamino)phenothiazin-10-yl]-3-(2,3dihydro-1H-cyclopenta[b]indol-4-yl)propan-1-one hydrochloride (14a), 1-[3,7-bis(dimethylamino)phenothiazin-10-yl]-3-(7-methyl-2,3-dihydro-1H-cyclopenta[b]indol-4-yl)propan-1-one (14b), 1-[3,7-bis(dimethylamino)phenothiazin-10-yl]-3-(1,2,3,4-tetrahydrocarbazol-9-yl)propan-1-one (15a), 1-[3,7-bis(dimethylamino)phenothiazin-10-yl]-3-(6-methyl-1,2,3,4-tetrahydrocarbazol-9-yl)propan-1-one (15b), 1-[3,7-bis(dimethylamino)phenothiazin-10-yl]-3-(6-fluoro-1,2,3,4-tetrahydrocarbazol-9-yl)propan-1-one (15c), 1-[3,7-bis(dimethylamino)phenothiazin-10-yl]-3-(6-methoxy-1,2,3,4-tetrahydrocarbazol-9-yl)propan-1-one (15d), 1-[3,7-bis(dimethylamino)phenothiazin-10-yl]-3-(6-trifluoromethoxy-1,2,3,4-tetrahydrocarbazol-9-yl)propan-1-one (15e), 1-[3,7-bis(dimethylamino)phenothiazin-10-yl]-3-(3-methyl-1,2,3,4-tetrahydrocarbazol-9-yl)propan-1-one (15f), 1-[3,7-bis(dimethylamino)phenothiazin-10-yl]-3-(3,6-dimethyl-1,2,3,4-tetrahydrocarbazol-9-yl)propan-1-one (15g), 1-[3,7-bis(dimethylamino)phenothiazin-10-yl]-3-(6-fluoro-3-methyl-1,2,3,4-tetrahydrocarbazol-9-yl)propan-1-one (15h), 1-[3,7-bis(dimethylamino)phenothiazin-10-yl]-3-(3-methyl-6-methoxy-1,2,3,4-tetrahydrocarbazol-9-yl)propan-1-one (15i), 1-[3,7-bis(dimethylamino)phenothiazin-10-yl]-3-(3methyl-6-trifluoromethoxy-1,2,3,4-tetrahydrocarbazol-9-yl)propan-1-one (15j), 1-[3,7-bis(dimethylamino)phenothiazin-10-yl]-3-(7,8,9,10-tetrahydro-6H-cyclohepta[b]indol-4-yl)propan-1-one (16a), 1-[3,7-bis(dimethylamino)phenothiazin-10-yl]-3-(2-methyl-7,8,9,10-tetrahydro-6H-cyclohepta[b]indol-4-yl)propan-1-one (16b), 1-[3,7-bis(dimethylamino)phenothiazin-10-yl]-3-(6,7,8,9,10,11-hexahydrocycloocta[b]indol-5-yl)propan-1-one (17a), 1-[3,7-bis(dimethylamino)phenothiazin-10-yl]-3-(2-methyl-6,7,8,9,10,11-hexahydrocycloocta[b]indol-5-yl)propan-1-one (17b).

The synthetic route of 13070-45-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Bachurin; Sokolov; Aksinenko; Epishina; Goreva; Gabre?yan; Grigo?ev; Russian Chemical Bulletin; vol. 64; 6; (2015); p. 1354 – 1361; Izv. Akad. Nauk, Ser. Khim.; 6; (2015); p. 1354 – 1361,7;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Extracurricular laboratory: Synthetic route of 13070-45-6

According to the analysis of related databases, 13070-45-6, the application of this compound in the production field has become more and more popular.

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 13070-45-6 as follows. HPLC of Formula: C13H15NO

Dissolve 93 mg of S11 in acetonitrile.Add 135 mg of 3,4-dihydroxybenzonitrile and add 7 mg of iron phthalocyanine under ice bath.30 mg of acetic acid, 4.8 mg of methanesulfonic acid and 135 mg of tert-butyl hydroperoxide, After stirring the reaction for 5 minutes under the same conditions,After monitoring the reaction, it was diluted with 20 mL of ethyl acetate and extracted with 20 mL of H2O.The combined organic layer Wash with 20 mL of saturated brine.Dry with anhydrous Na2SO4, filter and spin dry. Purified with silica gel column, eluent PE/ EtOAc = 8:1,188 mg of compound 11,The reaction yield was 56%;The product was a light yellow oil at room temperature.Physical state: light yellow oil; melting point: 138.5-139.4 C

According to the analysis of related databases, 13070-45-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Fuzhou University; Chen Haijun; Guo Mei; Ye Jinxiang; Chen Yi; Lin Yuqi; Gao Yu; (14 pag.)CN108530456; (2018); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Brief introduction of 13070-45-6

According to the analysis of related databases, 13070-45-6, the application of this compound in the production field has become more and more popular.

Application of 13070-45-6, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 13070-45-6 as follows.

General procedure: (S)-C10-BridgePHOS (2.0mg, 2.4mol%) and Pd(OCOCF3)2 (0.8mg, 2mol%) were placed into an oven dried flask under a nitrogen atmosphere, and degassed fresh dry acetone (2mL) was added. The mixture was stirred at room temperature for 1h. Then acetone was removed under vacuum and a solvent system of CH2Cl2/TFE (1/1, 1mL) was added to the mixture to afford the catalyst solution. The substrate 1 (0.15mmol) and additive (1equiv) were placed in a reaction tube under nitrogen and the above catalyst solution was added to the tube. The mixture was then degassed and transferred to a stainless steel autoclave in a glove box. After exchanging the gas three times, the hydrogenation was carried out at 35C under 60bar H2. After several hours, the reaction mixture was concentrated under reduced pressure. After alkalization with saturated NaHCO3, the percentage conversion of product was determined by 1H NMR analysis of the crude product. The organic residue was purified by flash chromatography with ethyl acetate/petrol ether (1:50) to give pure product 2. Enantiomeric excess was determined using a Daicel Chiralcel column with hexane/i-propyl alcohol as the eluant.

According to the analysis of related databases, 13070-45-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Li, Chao; Chen, Jianzhong; Fu, Guanghong; Liu, Delong; Liu, Yangang; Zhang, Wanbin; Tetrahedron; vol. 69; 33; (2013); p. 6839 – 6844;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem