Triethylamine → HCID 86644435、化合物

HRID 2404511ノート

反応式

HRID 2404511 の反応式
[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]

参加物

6

反応物 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 14474Perfluoro(methyl vinyl ether)HCID 178474353HCID 178474353、化合物

生成物 1

HCID 86644435HCID 86644435、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-f2cae7d38daf4deca495a7ea08682278
出典データセット
uspto-grants-2014_08
特許番号
US08802713B2

反応ノート

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