Water → 5-bromo-6-(4'-cyclohexylbenzyloxy)-3-ethyl-2-methylthio-4(3H)-pyrimidinone

HRID 1165204노트

반응식

HRID 1165204 반응식
[Br:1][C:2]1[C:3](=[O:13])[N:4]([CH2:11][CH3:12])[C:5]([S:9][CH3:10])=[N:6][C:7]=1[OH:8].[CH:14]1([C:20]2[CH:27]=[CH:26][C:23]([CH2:24]Cl)=[CH:22][CH:21]=2)[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[Br:1][C:2]1[C:3](=[O:13])[N:4]([CH2:11][CH3:12])[C:5]([S:9][CH3:10])=[N:6][C:7]=1[O:8][CH2:24][C:23]1[CH:26]=[CH:27][C:20]([CH:14]2[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19]2)=[CH:21][CH:22]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 133433651-(Chloromethyl)-4-cyclohexylbenzeneHCID 1360354175-bromo-3-ethyl-6-hydroxy-2-methylthio-4(3H)-pyrimidinone

생성물 1

HCID 142761825-bromo-6-(4'-cyclohexylbenzyloxy)-3-ethyl-2-methylthio-4(3H)-pyrimidinone수율 100%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

In 20 ml of N,N-dimethylformamide were dissolved 1 g of 5-bromo-3-ethyl-6-hydroxy-2-methylthio-4(3H)-pyrimidinone and 0.8 g of 4-cyclohexylbenzyl chloride, and then 1 g of anhydrous potassium carbonate was added thereto. The mixture was subjected to a reaction at 80° C. for 3 hours. After allowing to cool in air, the resulting solution was poured into 50 ml of water and extracted twice with 30 ml of ethyl ether. The ethyl ether layer was washed with water, dried over anhydrous sodium sulfate and then freed of solvent by distillation under reduced pressure to give 1.65 g of a crude product.

후처리

  1. customThe mixture was subjected to a reaction at 80° C. for 3 hours
  2. temperatureto cool in air
  3. extractionextracted twice with 30 ml of ethyl ether
  4. washThe ethyl ether layer was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationfreed of solvent by distillation under reduced pressure

출처 및 근거

ORD 기록
ord-327ddeef711c4e229ac43d89120d90bf
출처 데이터셋
uspto-grants-1990_03
특허 번호
US04908379

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