反応式
[CH3:1][N:2]([CH3:34])[CH2:3][CH2:4][N:5]1[C:9]2[CH:10]=[CH:11][C:12]([S:14]([C@@H:17]3[CH2:21][CH2:20][N:19](C(OC(C)(C)C)=O)[CH2:18]3)(=[O:16])=[O:15])=[CH:13][C:8]=2[N:7]=[C:6]1[CH2:29][C:30]([CH3:33])([CH3:32])[CH3:31].Cl[Si](C)(C)C>CO>[CH3:1][N:2]([CH3:34])[CH2:3][CH2:4][N:5]1[C:9]2[CH:10]=[CH:11][C:12]([S:14]([C@@H:17]3[CH2:21][CH2:20][NH:19][CH2:18]3)(=[O:15])=[O:16])=[CH:13][C:8]=2[N:7]=[C:6]1[CH2:29][C:30]([CH3:32])([CH3:31])[CH3:33]参加物
4
反応物 2
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 50 °C
実験手順
To a solution of (R)-tert-butyl 3-(1-(2-(dimethylamino)ethyl)-2-neopentyl-1H-benzo[d]imidazol-5-ylsulfonyl)pyrrolidine-1-carboxylate (STEP B, 612 mg, 1.24 mmol) in methanol (5 mL) was added chlorotrimethylsilane (749 microL, 6.21 mmol). The mixture was stirred at 50° C. for 3 h. The mixture was concentrated in vacuo. To the residue was added 2 mol/L sodium hydroxide aqueous solution to pH>7 and the mixture was extracted with ethyl acetate (150 mL). The organic layer was washed with brine and dried over sodium sulfate. The resulting solution was concentrated to give the title compound (453 mg, 93%) as an oil.
後処理
- concentrationThe mixture was concentrated in vacuo
- additionTo the residue was added 2 mol/L sodium hydroxide aqueous solution to pH>7
- extractionthe mixture was extracted with ethyl acetate (150 mL)
- washThe organic layer was washed with brine
- dry with materialdried over sodium sulfate
- concentrationThe resulting solution was concentrated
出典と根拠
- ORDレコード
- ord-d519c11abe5146429d739ddd8bed1bf6
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08653063B2
関連ノート
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