반응식
[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]참가 물질
4
반응물 2
생성물 1
시약·촉매·용매 1
반응 조건
- 온도
- 50 °C
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-d519c11abe5146429d739ddd8bed1bf6
- 출처 데이터셋
- uspto-grants-2014_02
- 특허 번호
- US08653063B2
연결된 노트
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