Triethylamine → HCID 86644435, 화합물

HRID 2404511노트

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HRID 2404511 반응식
[C:1]([NH:4][C:5]1[N:9]([C:10]2[CH:15]=[C:14]([S:16][CH2:17][C:18]([F:21])([F:20])[F:19])[C:13]([CH3:22])=[CH:12][C:11]=2[F:23])[N:8]=[C:7]([OH:24])[CH:6]=1)(=[O:3])[CH3:2].C(N(CC)CC)C.[F:32][C:33]([O:37][C:38]([F:41])([F:40])[F:39])=[C:34]([F:36])[F:35].C(OCC)(=O)C>CN(C)C=O>[C:1]([NH:4][C:5]1[N:9]([C:10]2[CH:15]=[C:14]([S:16][CH2:17][C:18]([F:19])([F:20])[F:21])[C:13]([CH3:22])=[CH:12][C:11]=2[F:23])[N:8]=[C:7]([O:24][C:34]([F:36])([F:35])[CH:33]([F:32])[O:37][C:38]([F:41])([F:40])[F:39])[CH:6]=1)(=[O:3])[CH3:2]

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 14474Perfluoro(methyl vinyl ether)HCID 178474353HCID 178474353, 화합물

생성물 1

HCID 86644435HCID 86644435, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

3.0 g of 5-acetylamino-1-{2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}-3-hydroxypyrazole was dissolved in 40 mL of dimethylformamide, 25 g of triethylamine was added, and stirring was carried out at 50° C. for 3 hours while trifluoromethyl trifluorovinyl ether was blown. To this solution, ethyl acetate was added, the solution was washed with a saturated aqueous solution of citric acid, the organic layer was dried over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure, and the obtained residue was purified by column chromatography (developing solvent ethyl acetate:hexane=1:4) to obtain 1.71 g of 5-acetylamino-1-{2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}-3-{1,1,2-trifluoro-2-(trifluoromethoxy)ethoxy}pyrazole.

후처리

  1. washthe solution was washed with a saturated aqueous solution of citric acid
  2. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  3. distillationthe solvent was distilled off under reduced pressure
  4. customthe obtained residue was purified by column chromatography (developing solvent ethyl acetate:hexane=1:4)

출처 및 근거

ORD 기록
ord-f2cae7d38daf4deca495a7ea08682278
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08802713B2

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