Chloroacetonitrile → 2-(3-Methoxyiminopyrrolidin-1-yl)-2-iminoethylchloride hydrochloride
반응식
[Cl:1][CH2:2][C:3]#[N:4].[Na].Cl.[CH3:7][O:8][N:9]=[C:10]1[CH2:14][CH2:13][NH:12][CH2:11]1>CO>[ClH:1].[CH3:7][O:8][N:9]=[C:10]1[CH2:14][CH2:13][N:12]([C:3](=[NH:4])[CH2:2][Cl:1])[CH2:11]1참가 물질
5
실험 절차
0.63 ml of chloroacetonitrile was added to a solution of 23 mg of metallic sodium in 4 ml of absolute methanol, the mixture was stirred at room temperature for about 30 minutes, then 1.5 g of 3-methoxyiminopyrrolidine hydrochloride were added and the resulting mixture stirred for a further 2 hours. After completion of the reaction, the solvent was distilled off and the concentrate mixed with anhydrous ether. The crystals which separated out were collected by filtration and washed with ether, giving 2.2 g of 2-(3-methoxyiminopyrrolidin-1-yl)-2-iminoethylchloride hydrochloride.
후처리
- stirringthe resulting mixture stirred for a further 2 hours
- customAfter completion of the reaction
- distillationthe solvent was distilled off
- additionthe concentrate mixed with anhydrous ether
- customThe crystals which separated out
- filtrationwere collected by filtration
- washwashed with ether
출처 및 근거
- ORD 기록
- ord-756d2cb4878d46e4a6c00d0a0fdbe11e
- 출처 데이터셋
- uspto-grants-1988_09
- 특허 번호
- US04771046
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