Ethyl 2-amino-4-phenylthiophene-3-carboxylate → Thieno(2,3-d)pyrimidin-4(1H)-one, 5-phenyl-

HRID 910180ノート

反応式

HRID 910180 の反応式
C([O:3][C:4]([C:6]1[C:10]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:9][S:8][C:7]=1[NH2:17])=O)C.C(O)(=O)C.[CH:22](N)=[NH:23]>C(O)C>[C:11]1([C:10]2[C:6]3[C:4](=[O:3])[NH:23][CH:22]=[N:17][C:7]=3[S:8][CH:9]=2)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

参加物

4

反応物 2

HCID 73242Ethyl 2-amino-4-phenylthiophene-3-carboxylateHCID 160693Formamidine acetate

生成物 1

HCID 215639Thieno(2,3-d)pyrimidin-4(1H)-one, 5-phenyl-

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A stirred mixture of 2-amino-4-phenylthiophene-3-carboxylic acid ethyl ester (350.43 g, 1.535 mol), formamidine acetate (799.13 g, 7.7 mol) and ethanol (1500 ml) was heated under reflux for 18 hours then allowed to cool to ambient temperature. The resulting solid was collected by filtration, washed with a little cold ethanol, then crystallised from ethanol to give 5-Phenyl-3H-thieno[2,3-d]pyrimidin-4-one as a yellow solid which was used without further purification.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 18 hours
  3. filtrationThe resulting solid was collected by filtration
  4. washwashed with a little cold ethanol
  5. customcrystallised from ethanol

出典と根拠

ORDレコード
ord-6e912309763f44a5a8a3d8b62049b509
出典データセット
uspto-grants-2011_09
特許番号
US08022076B2

反応ノート

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