Triethylamine → HCID 178498980、化合物

HRID 621422ノート

反応式

HRID 621422 の反応式
[NH2:1][C:2]([CH3:14])=[CH:3][C:4]([O:6][CH2:7][CH2:8][C:9]1[S:10][CH:11]=[CH:12][CH:13]=1)=[O:5].[N+:15]([C:18]1[CH:19]=[C:20]([CH:31]=[CH:32][CH:33]=1)[CH:21]=[C:22]([C:27](OC)=[O:28])[C:23]([O:25][CH3:26])=[O:24])([O-:17])=[O:16].C(N(CC)CC)C>CC(O)C>[OH:28][C:27]1[NH:1][C:2]([CH3:14])=[C:3]([C:4]([O:6][CH2:7][CH2:8][C:9]2[S:10][CH:11]=[CH:12][CH:13]=2)=[O:5])[CH:21]([C:20]2[CH:31]=[CH:32][CH:33]=[C:18]([N+:15]([O-:17])=[O:16])[CH:19]=2)[C:22]=1[C:23]([O:25][CH3:26])=[O:24]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 277557Dimethyl [(3-nitrophenyl)methylidene]propanedioateHCID 70042180HCID 70042180、化合物

生成物 1

HCID 178498980HCID 178498980、化合物収率 26.5%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A mixture of 2-(2-thienyl)ethyl 3-amino-2-butenoate (1.8 g) and dimethyl 3-nitrobenzylidenemalonate (2.25 g) was dissolved in anhydrous 2-propanol (80 ml) and, after addition of triethylamine (27 ml), the mixture was refluxed for 21 hours. After the solvent was distilled off under reduced pressure, the residue was purified by thin-layer silica gel chromatography (developing solvent: chloroform/methanol=19/1; elution solvent: chloroform/acetone=2/1) so as to obtain 1.0 g (26%) of the desired compound.

後処理

  1. temperaturethe mixture was refluxed for 21 hours
  2. distillationAfter the solvent was distilled off under reduced pressure
  3. customthe residue was purified by thin-layer silica gel chromatography (developing solvent: chloroform/methanol=19/1; elution solvent: chloroform/acetone=2/1) so as

出典と根拠

ORDレコード
ord-4787a4725a8343178e31938c9a9a0c99
出典データセット
uspto-grants-1989_04
特許番号
US04824837

反応ノート

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