These common heterocyclic compound, 10075-63-5, name is 1,5-Dimethoxynaphthalene, 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. Formula: C12H12O2
Methansulfonate 17. 5 part pentoxide diphosphorus 1. 75 part is added, with stirring at 23 C 30 minutes. The mixture obtained, eq. (I-44-a) compound represented by 3. 49 part is prepared, and then, is cooled to 0 C, eq. (I-44-b) compound represented by 5. 5 portion 92 by applying a dropped. After 20 minutes under stirring 0 C, further 23 C 18 at a time. The obtained reaction liquid is cooled to 0 C, ion exchange water 27. 03 part stocking, thereafter, 28% ammonia water 11. 07 by adding a neutralizing, represented by soln. contg. eq. (I-56) is obtained. A solution containing a salt eq. (I-56), eq. (I-44-c) compound represented by 7. 90 part and chloroform 78. 96 by adding, 24 hours at 23 C, a liquid. The organic layer, 40 parts of ion-exchanged water to mixing, stirring, liquid. This flush to 5 times. The organic layer, activated carbon 1. 00 part a, 30 minutes stirring at 23 C, filtration. The filtered liquid is concentrated, obtd. tert-butyl methyl ether 80 to the residue aminoacetonitrile 3 part is added and part, by concentrating the supernatant liquid is removed, the salt 7 eq. (I-44). 83 part is obtained.
The synthetic route of 1,5-Dimethoxynaphthalene has been constantly updated, and we look forward to future research findings.
Reference:
Patent; SUMITOMO CHEMICAL COMPANY LIMITED; ANRYU, YUKAKO; ICHIKAWA, KOJI; YOSHIDA, MASAFUMI; (86 pag.)JP2015/143208; (2015); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem