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

HRID 910181노트

반응식

HRID 910181 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-624b045e321143bb8448e982aa252e24
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08022076B2

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