반응식
[OH:1][C@H:2]1[CH2:7][CH2:6][N:5]([CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH2:4][C@H:3]1[C:15]([NH2:17])=O.B.CSC>C1COCC1>[NH2:17][CH2:15][C@H:3]1[C@@H:2]([OH:1])[CH2:7][CH2:6][N:5]([CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH2:4]1참가 물질
4
반응 조건
- 온도
- 80 °C
실험 절차
A solution of (cis)-4-hydroxy-1-(phenylmethyl)-3-piperidinecarboxamide (0.7 g, 3 mmol) in THF (6 ml) was treated with a borane-methyl sulphide complex (2M solution in THF, 3.3 ml). The reaction mixture was heated at 80° C. for 1300 s under microwave irradiation conditions. This was repeated twelve times and then the reaction mixtures were combined and the solvent was removed under reduced pressure and the residue was subjected to column chromatography on silica gel using a dichloromethane, methanol and aqueous ammonia gradient (20% methanol/dichloromethane-20% 2M ammonia in methanol/dichloromethane) to provide 4.6 g of the desired pure compound and 1.1 g of less pure material.
후처리
- customthe reaction mixtures
- customthe solvent was removed under reduced pressure
- customto provide 4.6 g of the desired pure compound and 1.1 g of less pure material
출처 및 근거
- ORD 기록
- ord-195aa1c634cc4890bc0ef7b3f3fc6293
- 출처 데이터셋
- uspto-grants-2010_06
- 특허 번호
- US07732461B2
연결된 노트
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