1-Methylpiperazine → Piperazine, 1-(3-butynyl)-4-methyl- (9CI)
반응식
CC1C=CC(S(O[CH2:12][CH2:13][C:14]#[CH:15])(=O)=O)=CC=1.[CH3:16][N:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1.C([O-])(O)=O.[Na+]>ClCCCl>[CH2:12]([N:20]1[CH2:21][CH2:22][N:17]([CH3:16])[CH2:18][CH2:19]1)[CH2:13][C:14]#[CH:15]참가 물질
5
반응 조건
- 온도
- 70 °C
실험 절차
A mixture of but-3-ynyl 4-methylbenzenesulfonate (972 mg) and N-methyl piperazine (482 μL) was heated to 80 C for 4.5 h, diluted with 1,2-dichloroethane (5 mL) and heated to 70° C. for 18 h. Saturated aq. NaHCO3 was added (10 mL) and the mixture was extracted with DCM (3×40 mL), and concentrated to afford 0.70 g of 1-(but-3-ynyl)-4-methylpiperazine as a 3:2 mixture of tosylate salt and free base.
후처리
- temperaturewas heated to 80 C for 4.5 h
- extractionthe mixture was extracted with DCM (3×40 mL)
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-bc2d2ada98c544b8a001f71f94e431e4
- 출처 데이터셋
- uspto-grants-2012_01
- 특허 번호
- US08093229B2
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