Water → 1-[(Benzoylamino)methyl]cyclohexanecarboxylic acid
반응식
[C:1]([NH:9][CH2:10][C:11]1([C:17]([O:19]CC)=[O:18])[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[K+].O>C(O)C>[C:1]([NH:9][CH2:10][C:11]1([C:17]([OH:19])=[O:18])[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1참가 물질
5
실험 절차
To a solution of ethyl 1-[(benzoylamino)methyl]cyclohexanecarboxylate (10.2 g, 35.1 mmol) in ethanol (50 ml) was added 50% aqueous potassium hydroxide solution (4 ml), and the mixture was heated under reflux for 6 hrs. Water (400 ml) was added and the reaction mixture was washed with diethyl ether. The aqueous layer was acidified (pH 2) with 5N hydrochloric acid, the precipitate was collected by filtration, washed with water and dried at 50° C. under reduced pressure. Recrystallization from ethanol-toluene gave the title compound (6.83 g, 74%) as colorless crystals.
후처리
- temperaturethe mixture was heated
- temperatureunder reflux for 6 hrs
- washthe reaction mixture was washed with diethyl ether
- filtrationthe precipitate was collected by filtration
- washwashed with water
- customdried at 50° C. under reduced pressure
- customRecrystallization from ethanol-toluene
출처 및 근거
- ORD 기록
- ord-e9f43d7980aa40c1bdaaed480f6a4600
- 출처 데이터셋
- uspto-grants-2011_07
- 특허 번호
- US07973163B2
반응 노트
불러오는 중…