Hydrazine hydrate (1:1) → Ethyl 5-(hydrazinecarboxamido)-3-methylthiophene-2-carboxylate
反応式
[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]参加物
4
実験手順
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).
後処理
- customThe resulting reaction mixture
- concentrationconcentrated in vacuo
- customThe residue was triturated with ethyl acetate
出典と根拠
- ORDレコード
- ord-d0f4d7d2d41040859ee0ead76e57f82e
- 出典データセット
- uspto-grants-2012_10
- 特許番号
- US08293768B2
反応ノート
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