반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([O:11][C@H:12]2[CH2:17][CH2:16][C@H:15]([C:18]3[CH:23]=[CH:22][C:21]([CH2:24][N:25]([CH3:27])[CH3:26])=[CH:20][CH:19]=3)[CH2:14][CH2:13]2)=[O:10])=[CH:4][CH:3]=1.Cl>C(OCC)C.C(O)(C)C>[ClH:1].[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([O:11][C@H:12]2[CH2:13][CH2:14][C@H:15]([C:18]3[CH:19]=[CH:20][C:21]([CH2:24][N:25]([CH3:26])[CH3:27])=[CH:22][CH:23]=3)[CH2:16][CH2:17]2)=[O:10])=[CH:4][CH:3]=1참가 물질
5
실험 절차
A solution of 0.39 g (0.001 mol) of trans-O-(4-chlorophenylacetyl)-4-(4-dimethylaminomethylphenyl)-cyclohexanol in 10 ml of diethyl ether is combined at ambient temperature, with stirring, with a 1.5 times equimolar amount of hydrogen chloride in isopropanol added dropwise. The precipitate formed is left for 1 hour at ambient temperature, suction filtered, washed repeatedly with diethyl ether and dried. White crystals are obtained, melting point 231-233° C. Yield: 0.32 g (76% of theory). C23H29Cl2NO2 (422.40) Calculated: C 65.40 H 6.92 N 3.32 Cl 16.79 Found: 65.33 7.06 3.45 16.92
후처리
- customis combined at ambient temperature
- additionadded dropwise
- customThe precipitate formed
- filtrationsuction filtered
- washwashed repeatedly with diethyl ether
- customdried
- customWhite crystals are obtained
출처 및 근거
- ORD 기록
- ord-73b2da3a71ba4351a5701078dc2ad8c9
- 출처 데이터셋
- uspto-grants-1999_10
- 특허 번호
- US05962507
연결된 노트
불러오는 중…