반응식
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][N:9]=2)[CH2:4][CH2:3]1.Cl[CH2:18][S:19]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)(=[O:21])=[O:20].CC([O-])(C)C.[K+]>C1COCC1>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[C:10]([CH2:18][S:19]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)(=[O:21])=[O:20])[N:9]=2)[CH2:4][CH2:3]1참가 물질
5
반응 조건
- 온도
- -10 °C
실험 절차
A stirred solution of 1-methyl-4-(5-nitropyridin-2-yl)piperazine (1.10 g, 5.00 mmol) and chloromethylphenylsulfone (0.950 g, 5.00 mmol) in dry THF, under nitrogen, is cooled to −60° C., treated with 1.0 M KOtBu in THF (10.0 mL, 10.0 mmol), allowed to warm to −10° C. over a 1 h period, quenched with acetic acid, treated sequentially with water and saturated aqueous NaHCO3 and extracted with CH2Cl2. The combined extracts are washed sequentially with water and brine, dried over MgSO4 and concentrated in vacuo. The resultant residue is crystallized from EtOAc to give the title compound as a yellow solid, 1.60 g (85% yield), mp: 170°-172° C., identified by mass spectral and NMR analyses.
후처리
- customquenched with acetic acid
- additiontreated sequentially with water and saturated aqueous NaHCO3
- extractionextracted with CH2Cl2
- washThe combined extracts are washed sequentially with water and brine
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
- customThe resultant residue is crystallized from EtOAc
출처 및 근거
- ORD 기록
- ord-b2b1b7e7168c4801a901b747bde79773
- 출처 데이터셋
- uspto-grants-2007_08
- 특허 번호
- US07259165B2
연결된 노트
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