Hydrazine hydrate (1:1) → Ethyl 5-(hydrazinecarboxamido)-3-methylthiophene-2-carboxylate
반응식
[CH3:1][C:2]1[CH:6]=[C:5]([NH:7][C:8](OC2C=CC=CC=2)=[O:9])[S:4][C:3]=1[C:17]([O:19][CH2:20][CH3:21])=[O:18].O.[NH2:23][NH2:24]>O1CCCC1>[NH:23]([C:8]([NH:7][C:5]1[S:4][C:3]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[C:2]([CH3:1])[CH:6]=1)=[O:9])[NH2:24]참가 물질
4
실험 절차
To a stirred suspension of ethyl 3-methyl-5-(phenoxycarbonylamino)-thiophene-2-carboxylate (18.89 g, 61.86 mmol) in tetrahydrofuran (130 mL) was added hydrazine monohydrate (19.0 mL, 391.7 mmol). The resulting reaction mixture was stirred for 2.5 h, and then concentrated in vacuo. The residue was triturated with ethyl acetate to afford ethyl 5-(hydrazinecarboxamido)-3-methylthiophene-2-carboxylate as a yellowish solid in 89% yield (13.30 g): MS (ES+) m/z 244.2 (M+1).
후처리
- customThe resulting reaction mixture
- concentrationconcentrated in vacuo
- customThe residue was triturated with ethyl acetate
출처 및 근거
- ORD 기록
- ord-d0f4d7d2d41040859ee0ead76e57f82e
- 출처 데이터셋
- uspto-grants-2012_10
- 특허 번호
- US08293768B2
반응 노트
불러오는 중…