Methyl 5-(2,4-dimethoxybenzylamino)-4-nitrothiophene-2-carboxylate → Methyl 5-amino-4-nitrothiophene-2-carboxylate
反応式
COC1C=C(OC)C=CC=1C[NH:6][C:7]1[S:11][C:10]([C:12]([O:14][CH3:15])=[O:13])=[CH:9][C:8]=1[N+:16]([O-:18])=[O:17]>C(Cl)Cl.C(O)(C(F)(F)F)=O>[NH2:6][C:7]1[S:11][C:10]([C:12]([O:14][CH3:15])=[O:13])=[CH:9][C:8]=1[N+:16]([O-:18])=[O:17]参加物
4
実験手順
A solution of methyl 5-(2,4-dimethoxybenzylamino)-4-nitrothiophene-2-carboxylate 86 (40.3 mmol, 14.2 g) in CH2Cl2 (100 mL) and TFA (10 mL) was stirred overnight at rt. Reaction mixture was poured on ice and the precipitate was collected to give methyl 5-amino-4-nitrothiophene-2-carboxylate 87 (8.15 g, 100%). NMR (400 MHz, DMSO-d6) 3.77 (s, 3H), 7.75 (s, 1H), 9.06 (br s, 2H).
後処理
- customReaction mixture
- additionwas poured on ice
- customthe precipitate was collected
出典と根拠
- ORDレコード
- ord-3e4ee040543d4e9fb457956a0816bcf5
- 出典データセット
- uspto-grants-2014_03
- 特許番号
- US08669256B2
反応ノート
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