Water → HCID 19932136、化合物

HRID 21607ノート

反応式

HRID 21607 の反応式
C(N(S(F)(F)[F:7])CC)C.[CH2:10]([N:12]([CH2:33][CH3:34])[C:13]([N:15]1[CH:19]=[C:18]([CH2:20]O)[C:17]([S:22]([C:25]2[CH:30]=[CH:29][CH:28]=[C:27]([Cl:31])[C:26]=2[CH3:32])(=[O:24])=[O:23])=[N:16]1)=[O:14])[CH3:11].O>C(Cl)Cl>[CH2:10]([N:12]([CH2:33][CH3:34])[C:13]([N:15]1[CH:19]=[C:18]([CH2:20][F:7])[C:17]([S:22]([C:25]2[CH:30]=[CH:29][CH:28]=[C:27]([Cl:31])[C:26]=2[CH3:32])(=[O:24])=[O:23])=[N:16]1)=[O:14])[CH3:11]

参加物

5

反応物 3

HCID 962WaterHCID 123472(Diethylamino)sulfur trifluorideHCID 19931990HCID 19931990、化合物

生成物 1

HCID 19932136HCID 19932136、化合物収率 95%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

20 μl of diethylaminosulfur trifluoride were added at 0° C. to a solution of 54 mg of 1-(diethylcarbamoyl)-3-(2-methyl-3-chlorophenylsulfonyl)-4-hydroxymethylpyrazole (prepared as described in Example 10) in 1.8 ml of methylene chloride, and the resulting mixture was stirred for 1 hour. At the end of this time, the reaction mixture was poured into water and extracted with methylene chloride. The extract was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate and concentrated by evaporation under reduced pressure. The concentrate was purified by column chromatography through silica gel, eluted with an 8:1 by volume mixture of hexane and ethyl acetate, to afford 51 mg (yield 95%) of the title compound as an oil.

後処理

  1. extractionextracted with methylene chloride
  2. washThe extract was washed with a saturated aqueous solution of sodium chloride
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated by evaporation under reduced pressure
  5. customThe concentrate was purified by column chromatography through silica gel
  6. washeluted with an 8:1 by volume mixture of hexane and ethyl acetate

出典と根拠

ORDレコード
ord-3e37884e66614bbc968e7efc33694788
出典データセット
uspto-grants-1995_06
特許番号
US05424279

反応ノート

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