Water → N-cyclopropylpyridin-4-amine
반응식
Cl[C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[CH:15]1([NH2:18])[CH2:17][CH2:16]1.O>CN(C=O)C>[CH:15]1([NH:18][C:2]2[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=2)[CH2:17][CH2:16]1참가 물질
6
실험 절차
To a magnetically stirred, 25° C. solution of 2.3 g (0.006 mol) of product of Step A and 0.71 g (0.007 mol) of triethylamine in 40 ml of DMF was added dropwise 0.38 g (0.007 mol) of cyclopropylamine. After 18 hours the reaction mixture was poured into H2O and extracted with diethyl ether. The ether phase was washed with H2O, and dried (MgSO4). The dry ether phase was concentrated in vacuo to 1.95 g of a brown solid. The crude was recrystallized from hexane/EtOAc affording 1.2 g (50%) of product as a beige solid; mp 111°-112° C.
후처리
- extractionextracted with diethyl ether
- washThe ether phase was washed with H2O
- dry with materialdried (MgSO4)
- concentrationThe dry ether phase was concentrated in vacuo to 1.95 g of a brown solid
- customThe crude was recrystallized from hexane/EtOAc affording 1.2 g (50%) of product as a beige solid
출처 및 근거
- ORD 기록
- ord-15b07f6687274474a60864e8a80251c3
- 출처 데이터셋
- uspto-grants-1990_05
- 특허 번호
- US04921530
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