3,3-Dimethylbutylamine → 3-[Benzyl-(1-phenyl-ethyl)-amino]-3-cyclohexyl-N-(3,3-dimethyl-butyl)-propionamide
反応式
[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]=1参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-af8bd0aa04bb4220bbd2cfb89723f51d
- 出典データセット
- uspto-grants-2009_05
- 特許番号
- US07531545B2
反応ノート
読み込み中…