Thionyl Chloride → 2-Chloromethyl-4-dimethylaminomethylpyridine hydrochloride
반응식
[CH3:1][N:2]([CH2:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]([CH2:11]O)[CH:6]=1)[CH3:3].S(Cl)([Cl:15])=O>ClCCl>[ClH:15].[Cl:15][CH2:11][C:7]1[CH:6]=[C:5]([CH2:4][N:2]([CH3:3])[CH3:1])[CH:10]=[CH:9][N:8]=1참가 물질
4
실험 절차
4-Dimethylaminomethyl-2-hydroxymethylpyridine (13.45 g) in dichloromethane (200 ml) was added dropwise to a stirred solution of thionyl chloride (30 ml) in dichloromethane (150 ml). The resulting red mixture was stirred for 1 hour then concentrated in vacuo. The residue was treated with ether (300 ml) to yield a crystalline solid. Recrystallisation from methanol/ether (1:3) yielded 2-chloromethyl-4-dimethylaminomethylpyridine hydrochloride (20.04 g) as an orange solid m.p. 202°-204°.
후처리
- concentrationthen concentrated in vacuo
- additionThe residue was treated with ether (300 ml)
- customto yield a crystalline solid
- customRecrystallisation from methanol/ether (1:3)
출처 및 근거
- ORD 기록
- ord-f8f3eae858ce4961aef0a298790c4aa1
- 출처 데이터셋
- uspto-grants-1984_03
- 특허 번호
- US04439609
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