Triethylamine → Methyl 4-(ethoxycarbonylamino)-thiophene-3-carboxylate
反応式
Cl.[NH2:2][C:3]1[C:4]([C:8]([O:10][CH3:11])=[O:9])=[CH:5][S:6][CH:7]=1.C(N(CC)CC)C.[C:19](Cl)(=[O:23])[O:20][CH2:21][CH3:22]>C1(C)C=CC=CC=1>[CH2:21]([O:20][C:19]([NH:2][C:3]1[C:4]([C:8]([O:10][CH3:11])=[O:9])=[CH:5][S:6][CH:7]=1)=[O:23])[CH3:22]参加物
5
実験手順
A mixture of 50.0 g (0.258 mol) of methyl 4-aminothiophen-3-carboxylate-hydrochloride, 700 ml of toluene, 26 g (0.257 mol) of triethylamine and 27 ml (0.283 mol) of ethyl chlorocarbonate was refluxed for 5 hours. The insoluble matter was filtered off, the filtrate was evaporated down in vacuo and the residue was crystallised from petroleum ether. 59.0 g (99.8% of theory) of colourless crystals of melting point 52° C. were obtained.
後処理
- temperaturewas refluxed for 5 hours
- filtrationThe insoluble matter was filtered off
- customthe filtrate was evaporated down in vacuo
- customthe residue was crystallised from petroleum ether
- custom59.0 g (99.8% of theory) of colourless crystals of melting point 52° C. were obtained
出典と根拠
- ORDレコード
- ord-4dee884051634d85978fb60409e5c8dd
- 出典データセット
- uspto-grants-2009_03
- 特許番号
- US07498325B2
反応ノート
読み込み中…