Ethyl formate → 5-(N-formylamino)-valeric acid ethyl ester
반응식
C(N(CC)CC)C.Cl.[CH2:9]([O:11][C:12](=[O:18])[CH2:13][CH2:14][CH2:15][CH2:16][NH2:17])[CH3:10].[CH2:19]([O:21]C=O)C>>[CH2:9]([O:11][C:12](=[O:18])[CH2:13][CH2:14][CH2:15][CH2:16][NH:17][CH:19]=[O:21])[CH3:10]참가 물질
4
실험 절차
1.4 ml of triethylamine are added to 1.8 g of 5-aminovaleric acid ethyl ester hydrochloride in 40 ml of formic acid ethyl ester and the whole is then heated under reflux for 2 hours. The precipitate is filtered off, washed with a small quantity of formic acid ethyl ester and concentrated by evaporation under reduced pressure in a rotary evaporator. The residue is partitioned between methylene chloride and sodium bicarbonate solution, and the organic phase is then washed with brine, dried and concentrated by evaporation. The title compound is obtained in the form of an oil.
후처리
- temperaturethe whole is then heated
- temperatureunder reflux for 2 hours
- filtrationThe precipitate is filtered off
- washwashed with a small quantity of formic acid ethyl ester
- concentrationconcentrated by evaporation under reduced pressure in a rotary evaporator
- customThe residue is partitioned between methylene chloride and sodium bicarbonate solution
- washthe organic phase is then washed with brine
- customdried
- concentrationconcentrated by evaporation
출처 및 근거
- ORD 기록
- ord-1ec757bc98004f3490119112f063295b
- 출처 데이터셋
- uspto-grants-1988_12
- 특허 번호
- US04794109
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