Acetone Cyanohydrin → HCID 178463113, 화합물

HRID 1857324

반응식

HRID 1857324 반응식
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]

참가 물질

6

반응물 4

HCID 6406Acetone CyanohydrinHCID 8471Triethylamine2회HCID 22129431HCID 22129431, 화합물HCID 178463041HCID 178463041, 화합물

생성물 1

HCID 178463113HCID 178463113, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-243ab9a9659348e398e39911fd9e8f5c
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06147031

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