Acetone Cyanohydrin → HCID 178463113、化合物

HRID 1857324

反応式

HRID 1857324 の反応式
Cl.[CH2:2]([N:4]1[C:8]([OH:9])=[CH:7][CH:6]=[N:5]1)[CH3:3].C(N(CC)CC)C.[O:17]1[CH:21]=[CH:20][C:19]([C:22]2[C:23]([CH3:35])=[C:24]([CH:28]=[CH:29][C:30]=2[S:31]([CH3:34])(=[O:33])=[O:32])[C:25](Cl)=[O:26])=[N:18]1.CC(C)(O)C#N>C(Cl)(Cl)Cl>[CH2:2]([N:4]1[C:8]([OH:9])=[C:7]([C:25](=[O:26])[C:24]2[CH:28]=[CH:29][C:30]([S:31]([CH3:34])(=[O:33])=[O:32])=[C:22]([C:19]3[CH:20]=[CH:21][O:17][N:18]=3)[C:23]=2[CH3:35])[CH:6]=[N:5]1)[CH3:3]

参加物

6

反応物 4

HCID 6406Acetone CyanohydrinHCID 8471Triethylamine2 回HCID 22129431HCID 22129431、化合物HCID 178463041HCID 178463041、化合物

生成物 1

HCID 178463113HCID 178463113、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

Separately 0.38 g of 1-ethyl-5-hydroxypyrazole hydrochloride was dissolved in 10 ml of chloroform, and 0.52 g of triethylamine was added, while cooling with ice. Into the obtained solution was added dropwise 5 ml of a chloroform solution containing the previously obtained 3-(isoxazol-3-yl)-4-methylsulfonyl-2-methylbenzoyl chloride to stir at room temperature for an hour. To the reaction mixture were added 0.26 g of triethylamine and 0.05 g of acetone cyanohydrin to further stir overnight. The reaction solution was washed with dilute hydrochloric acid, with water, then with a saturated sodium chloride solution, and dried over anhydrous magnesium sulfate. The solvent was distilled out under reduced pressure. Methanol was added to the obtained residue. The produced crystals were separated by filtration to give 0.18 g of the title compound as white crystals. m.p. 85~88° C.

後処理

  1. temperaturewhile cooling with ice
  2. washThe reaction solution was washed with dilute hydrochloric acid, with water
  3. dry with materialwith a saturated sodium chloride solution, and dried over anhydrous magnesium sulfate
  4. distillationThe solvent was distilled out under reduced pressure
  5. additionMethanol was added to the obtained residue
  6. customThe produced crystals were separated by filtration

出典と根拠

ORDレコード
ord-243ab9a9659348e398e39911fd9e8f5c
出典データセット
uspto-grants-2000_11
特許番号
US06147031

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