Acetamidine monohydrochloride → 2-methyl-5-phenyl-3H-thieno[2,3-d]pyrimidin-4-one

HRID 910181ノート

反応式

HRID 910181 の反応式
C(O[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:5])C.Cl.[C:19](N)(=[NH:21])[CH3:20]>C(O)C>[CH3:20][C:19]1[NH:21][C:4](=[O:5])[C:6]2[C:10]([C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=3)=[CH:9][S:8][C:7]=2[N:17]=1

参加物

4

反応物 2

HCID 67170Acetamidine monohydrochlorideHCID 73242Ethyl 2-amino-4-phenylthiophene-3-carboxylate

生成物 1

HCID 7145082-methyl-5-phenyl-3H-thieno[2,3-d]pyrimidin-4-one

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, 1.54 mol), acetamidine hydrochloride (725.13 g, 7.676 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 2-Methyl-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-624b045e321143bb8448e982aa252e24
出典データセット
uspto-grants-2011_09
特許番号
US08022076B2

反応ノート

読み込み中…