반응 #5875

반응 방정식

2,3-dihydro-3-methyl-1H-inden-1-one

methyl 2-aminoacetate

thiophene

sodium formate

→

methyl N-(2,3-dihydro-3-methyl-1H-inden-1-yl)glycine

수율 54.1%

용매

methanol

methanol

반응 조건

후처리

1. 1
   기타The reaction mixture is evaporated
2. 2
   workup.ADDITION1,1'-oxybisethane is added
3. 3
   추출The separated organic layer is extracted with a hydrochloric acid solution 10%
4. 4
   추출the product is extracted with 1,1'-oxybisethane
5. 5
   기타The combined extracts are dried
6. 6
   여과filtered
7. 7
   기타evaporated

실험 절차

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.

출처