Potassium Carbonate → ethyl 4-(2-chlorophenyl)-2-[5-(trifluoromethyl)-2H-tetrazol-2-yl]methylpyrimidine-5-carboxylate

HRID 1958085노트

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HRID 1958085 반응식
Br[CH2:2][C:3]1[N:8]=[C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[Cl:15])[C:6]([C:16]([O:18][CH2:19][CH3:20])=[O:17])=[CH:5][N:4]=1.[F:21][C:22]([C:25]1[NH:29][N:28]=[N:27][N:26]=1)([F:24])[F:23].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[Cl:15][C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=1[C:7]1[C:6]([C:16]([O:18][CH2:19][CH3:20])=[O:17])=[CH:5][N:4]=[C:3]([CH2:2][N:27]2[N:28]=[N:29][C:25]([C:22]([F:24])([F:23])[F:21])=[N:26]2)[N:8]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 67125220HCID 67125220, 화합물HCID 178506305HCID 178506305, 화합물

생성물 1

HCID 67125210ethyl 4-(2-chlorophenyl)-2-[5-(trifluoromethyl)-2H-tetrazol-2-yl]methylpyrimidine-5-carboxylate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
60 °C

실험 절차

An amount of 345 mg (0.97 mmol) of ethyl 2-(bromomethyl)-4-(2-chlorophenyl)pyrimidine-5-carboxylate was added to a solution of 200 mg (1.45 mmol) of trifluoromethyltetrazole in 10 ml of acetonitrile. Then 174 mg (1.26 mmol) of potassium carbonate were added to the reaction solution, which was stirred at 60° C. for 6 hours. After cooling to room temperature, the reaction solution was filtered and the mother liquor was freed from the solvent under reduced pressure. The residue was admixed with 10 ml of water and extracted with ethyl acetate (3×20 ml). The combined organic phases were dried over sodium sulphate. The solvent was removed under reduced pressure and the residue was purified by chromatography.

후처리

  1. temperatureAfter cooling to room temperature
  2. filtrationthe reaction solution was filtered
  3. extractionextracted with ethyl acetate (3×20 ml)
  4. dry with materialThe combined organic phases were dried over sodium sulphate
  5. customThe solvent was removed under reduced pressure
  6. customthe residue was purified by chromatography

출처 및 근거

ORD 기록
ord-7d6394b6fd4f4fd3bb5031294da3bcdb
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08410106B2

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