Methyl iodide → 3-(4-Bromo-5-ethoxy-2-fluorophenyl)-1-methyl-6-trifluoromethyl-2,4(1h,3h)-pyrimidinedione

HRID 566182노트

반응식

HRID 566182 반응식
[Br:1][C:2]1[C:7]([O:8][CH2:9][CH3:10])=[CH:6][C:5]([N:11]2[C:16](=[O:17])[CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[NH:13][C:12]2=[O:22])=[C:4]([F:23])[CH:3]=1.CI.[C:26](=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Br:1][C:2]1[C:7]([O:8][CH2:9][CH3:10])=[CH:6][C:5]([N:11]2[C:16](=[O:17])[CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[N:13]([CH3:26])[C:12]2=[O:22])=[C:4]([F:23])[CH:3]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 212655333-(4-Bromo-5-ethoxy-2-fluorophenyl)-6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione

생성물 1

HCID 110801123-(4-Bromo-5-ethoxy-2-fluorophenyl)-1-methyl-6-trifluoromethyl-2,4(1h,3h)-pyrimidinedione수율 84.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

3-(4-Bromo-5-ethoxy-2-fluorophenyl)-6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione (2.38 g), methyl iodide (1.06 g) and potassium carbonate (1.04 g) were suspended in DMF (12 ml), and the mixture was stirred at room temperature for about 8 hours. After the reaction, DMF was distilled off under reduced pressure, extracted with ethyl acetate, washed with water, and dried over anhydrous magnesium sulfate. Then, ethyl acetate was distilled off, and the resulting residue was crystallized from a mixed solvent of ethyl acetate and n-hexane (1:5 v/v) to obtain the objective 3-(4-bromo-5-ethoxy-2-fluorophenyl)-1-methyl-6-trifluoromethyl-2,4( 1H,3H)-pyrimidinedione (2.08 g).

후처리

  1. distillationwas distilled off under reduced pressure
  2. extractionextracted with ethyl acetate
  3. washwashed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationThen, ethyl acetate was distilled off
  6. customthe resulting residue was crystallized from a mixed solvent of ethyl acetate and n-hexane (1:5 v/v)

출처 및 근거

ORD 기록
ord-ef6aaa9530ca4b3a8a382ef03a20afbf
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06174839B1

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