Water → HCID 19931990、化合物

HRID 21606ノート

反応式

HRID 21606 の反応式
[BH4-].[Na+].[CH2:3]([N:5]([CH2:26][CH3:27])[C:6]([N:8]1[CH:12]=[C:11]([CH:13]=[O:14])[C:10]([S:15]([C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([Cl:24])[C:19]=2[CH3:25])(=[O:17])=[O:16])=[N:9]1)=[O:7])[CH3:4].O>CO>[CH2:26]([N:5]([CH2:3][CH3:4])[C:6]([N:8]1[CH:12]=[C:11]([CH2:13][OH:14])[C:10]([S:15]([C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([Cl:24])[C:19]=2[CH3:25])(=[O:17])=[O:16])=[N:9]1)=[O:7])[CH3:27]

参加物

5

反応物 3

HCID 962WaterHCID 4311764Sodium borohydrideHCID 199319281-(Diethylcarbamoyl)-3-(2-methyl-3-chlorophenylsulfonyl)-4-formylpyrazole

生成物 1

HCID 19931990HCID 19931990、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

11 mg of sodium borohydride were added at 0° C. to a solution of 112 mg of 1-(diethylcarbamoyl)-3-(2-methyl-3-chlorophenylsulfonyl)-4-formylpyrazole [prepared as described in Example 9(3)] in 3.5 ml of methanol, and the resulting mixture was stirred for 30 minutes. At the end of this time, the reaction mixture was poured into water and extracted with ethyl acetate. 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 a 5:1 by volume mixture of hexane and ethyl acetate, to afford 114 mg (a quantitative yield) of the title compound as an oil.

後処理

  1. extractionextracted with ethyl acetate
  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 a 5:1 by volume mixture of hexane and ethyl acetate

出典と根拠

ORDレコード
ord-f8abc9b5745740e9b329aee1eeb3172f
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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