1,1-Bis(2,2-dimethylpropoxy)-N,N-dimethylmethanamine → 1-(5-Bromothien-2-ylmethyl)-5-chloropyrimidin-2-one

HRID 434655노트

반응식

HRID 434655 반응식
C(OC(OCC(C)(C)C)N(C)C)C(C)(C)C.[Cl:17][C:18]1[CH:19]=[N:20][C:21](=[O:24])[NH:22][CH:23]=1.[Br:25][C:26]1[S:30][C:29]([CH2:31]O)=[CH:28][CH:27]=1>CN(C)C=O>[Br:25][C:26]1[S:30][C:29]([CH2:31][N:20]2[CH:19]=[C:18]([Cl:17])[CH:23]=[N:22][C:21]2=[O:24])=[CH:28][CH:27]=1

참가 물질

5

반응물 3

HCID 786231,1-Bis(2,2-dimethylpropoxy)-N,N-dimethylmethanamineHCID 1085785-Chloro-2(1H)-pyrimidinoneHCID 11435467(5-Bromothiophen-2-yl)methanol

생성물 1

HCID 204917611-(5-Bromothien-2-ylmethyl)-5-chloropyrimidin-2-one수율 45.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
40 °C

실험 절차

N,N-Dimethylformamide dineopentyl acetal (2.25 ml) was added to a stirred suspension of 5-chloropyrimidin-2-one (653 mg) and 5-bromo-2-hydroxymethylthiophene (1.351 g) in dry N,N-dimethylformamide (12.5 ml) under nitrogen and then the mixture was heated at 40° C. After 2 h the temperature was increased to 80° C. After 4 h the reaction mixture was evaporated to dryness and the residue triturated with diethyl ether. The solid was collected and crystallised from acetone to give off white crystals of the title pyrimidinone (691 mg), m.p. 217°-220° C., λmax (EtOH) 243.5 nm (ε 13,810), 336 nm (ε 1,190).

후처리

  1. temperatureAfter 2 h the temperature was increased to 80° C
  2. customAfter 4 h the reaction mixture was evaporated to dryness
  3. customthe residue triturated with diethyl ether
  4. customThe solid was collected
  5. customcrystallised from acetone

출처 및 근거

ORD 기록
ord-8983776e7a9a42ca87ea3ed0d4d526b3
출처 데이터셋
uspto-grants-1983_08
특허 번호
US04399140

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