3,3-Dimethylbutylamine → 3-[Benzyl-(1-phenyl-ethyl)-amino]-3-cyclohexyl-N-(3,3-dimethyl-butyl)-propionamide
반응식
[CH3:1][C:2]([CH3:7])([CH3:6])[CH2:3][CH2:4][NH2:5].[CH2:8]([N:15]([CH:27]([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[CH3:28])[CH:16]([CH:21]1[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1)[CH2:17][C:18](O)=[O:19])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C>CN(C=O)C>[CH2:8]([N:15]([CH:27]([C:29]1[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=1)[CH3:28])[CH:16]([CH:21]1[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1)[CH2:17][C:18]([NH:5][CH2:4][CH2:3][C:2]([CH3:7])([CH3:6])[CH3:1])=[O:19])[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1참가 물질
6
반응물 4
생성물 1
시약·촉매·용매 1
실험 절차
A mixture of 3,3-dimethyl butylamine (0.6 mL, 4.2 mmol), 3-[benzyl-(1-phenyl-ethyl)-amino]-3-cyclohexyl-propionic acid (1.83 g, 3.8 mmol), HBTU (2.2 g, 5.7 mmol), DIPEA (1.5 mL, 8.6 mmol) and DMF (25 mL) was stirred at room temperature for 14 hours. To the reaction mixture was then added sodium bicarbonate(s) (100 mL) and the desired product was extracted with ethyl acetate (100 mL×2). The combined organic layers were washed with water, dried over MgSO4 and concentrated to yield a solid. The solid was purified by column chromatography (10% EtOAc/heptane) to yield a residue.
후처리
- extractionadded sodium bicarbonate(s) (100 mL) and the desired product was extracted with ethyl acetate (100 mL×2)
- washThe combined organic layers were washed with water
- dry with materialdried over MgSO4
- concentrationconcentrated
- customto yield a solid
- customThe solid was purified by column chromatography (10% EtOAc/heptane)
- customto yield a residue
출처 및 근거
- ORD 기록
- ord-af8bd0aa04bb4220bbd2cfb89723f51d
- 출처 데이터셋
- uspto-grants-2009_05
- 특허 번호
- US07531545B2
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