Water → HCID 11524380, 화합물

HRID 1348993

반응식

HRID 1348993 반응식
[CH3:1][O:2][C:3]1[C:4](S(C)(=O)=O)=[N:5][C:6]([N:9]2[CH:13]=[C:12]([C:14]([F:17])([F:16])[F:15])[CH:11]=[N:10]2)=[N:7][CH:8]=1.[OH:22][C:23]1[CH:27]=[C:26]([C:28]([F:31])([F:30])[F:29])[S:25][CH:24]=1.C([O-])([O-])=O.[K+].[K+].O>CN(C=O)C>[CH3:1][O:2][C:3]1[C:4]([O:22][C:23]2[CH:27]=[C:26]([C:28]([F:31])([F:30])[F:29])[S:25][CH:24]=2)=[N:5][C:6]([N:9]2[CH:13]=[C:12]([C:14]([F:15])([F:16])[F:17])[CH:11]=[N:10]2)=[N:7][CH:8]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 110842734-Hydroxy-2-(trifluoromethyl)thiopheneHCID 12115990HCID 12115990, 화합물

생성물 1

HCID 11524380HCID 11524380, 화합물수율 59%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

A mixture of 0.4 g (1.24 mmol) of 5-methoxy-4-methylsulfonyl-2-(4-trifluoromethyl-1H-1-pyrazolyl)pyrimidine, 0.27 g (1.60 mmol) of 3-hydroxy-5-trifluoromethyl-thiophene and 0.34 g (2.47 mmol) of K2CO3 in 10 ml of DMF is stirred at 60° C. for 6 h and then at RT for 48 h. It is subsequently poured into 20 ml of water and extracted with four times 15 ml of CH2Cl2. The combined organic phase is dried over Na2SO4, filtered and concentrated. Chromatographic purification on silica gel with heptane/ethyl acetate (3:7) as eluent gives 0.3 g of 5-methoxy-2-(4-trifluoromethyl-1H-1-pyrazolyl)-4-(5-trifluoromethyl-3-thienyloxy)pyrimidine as colorless crystals.

후처리

  1. waitat RT for 48 h
  2. extractionextracted with four times 15 ml of CH2Cl2
  3. dry with materialThe combined organic phase is dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customChromatographic purification on silica gel with heptane/ethyl acetate (3:7) as eluent

출처 및 근거

ORD 기록
ord-c1671ce1ad6b441c8f8873f2c82ce678
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07211673B2

연결된 노트

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