HRID5779

反应详情

EQUATION

反应方程式

HRID 5779 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 21 parts of 2,3-dihydro-3-methyl-1H-inden-1-one, 25 parts of methyl 2-aminoacetate, 2 parts of a solution of thiophene in methanol 4%, 25 parts of sodium formate and 480 parts of methanol is hydrogenated in a Parr-apparatus and at 50° C. with 5 parts of palladium-on-charcoal catalyst 10%. The reaction mixture is evaporated. The residue is taken up in water and 1,1'-oxybisethane is added. The separated organic layer is extracted with a hydrochloric acid solution 10%. The aqueous layer is made alkaline and the product is extracted with 1,1'-oxybisethane. The combined extracts are dried, filtered and evaporated, yielding 19 parts (54.1%) of methyl N-(2,3-dihydro-3-methyl-1H-inden-1-yl)glycine as a residue.

WORKUP

后处理

  1. customThe reaction mixture is evaporated
  2. addition1,1'-oxybisethane is added
  3. extractionThe separated organic layer is extracted with a hydrochloric acid solution 10%
  4. extractionthe product is extracted with 1,1'-oxybisethane
  5. customThe combined extracts are dried
  6. filtrationfiltered
  7. customevaporated