반응식
[OH:1][CH2:2][C@@H:3]1[NH:8][CH2:7][CH2:6][N:5]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:4]1.C=O.[C:18](O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])[O-].[Na+].[Na+]>C(#N)C.O.C(Cl)Cl.CO>[OH:1][CH2:2][C@@H:3]1[N:8]([CH3:18])[CH2:7][CH2:6][N:5]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:4]1참가 물질
반응물 4
생성물 1
시약·촉매·용매 4
실험 절차
To a solution of (R)-tert-butyl 3-(hydroxymethyl)piperazine-1-carboxylate (115 mg, 0.53 mmol) in acetonitrile (1.4 mL) and water (0.3 mL) was added Formalin (0.11 mL, 1.6 mmol) followed by sodium triacetoxyborohydride (225 mg, 1.1 mmol). The reaction mixture was stirred for 20 minutes at ambient temperature. The reaction mixture was then basified via the addition of saturated aqueous sodium carbonate solution (1 mL), diluted with methylene chloride (50 mL) and methanol (5 mL), and washed with saturated aqueous sodium bicarbonate solution (2×15 mL). The organic layer was separated, dried over sodium sulfate, and concentrated in vacuo to afford a white crystalline solid, which was used in the next step without any further purification (120 mg, 98%).
후처리
- washwashed with saturated aqueous sodium bicarbonate solution (2×15 mL)
- customThe organic layer was separated
- dry with materialdried over sodium sulfate
- concentrationconcentrated in vacuo
- customto afford a white crystalline solid, which
- customwas used in the next step without any further purification (120 mg, 98%)
출처 및 근거
- ORD 기록
- ord-209d4574534a4c8dbaebce40c777f396
- 출처 데이터셋
- uspto-grants-2016_09
- 특허 번호
- US09440976B2
연결된 노트
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