Phenacyl bromide → 4-[3-(4,5-Dihydroisoxazol-3-yl)-4-methylsulfonyl-2-methylbenzoyl]-1-ethyl-5-phenacyloxypyrazole

HRID 1857322

반응식

HRID 1857322 반응식
[O:1]1[CH2:5][CH2:4][C:3]([C:6]2[C:7]([CH3:26])=[C:8]([CH:19]=[CH:20][C:21]=2[S:22]([CH3:25])(=[O:24])=[O:23])[C:9]([C:11]2[CH:12]=[N:13][N:14]([CH2:17][CH3:18])[C:15]=2[OH:16])=[O:10])=[N:2]1.C(=O)([O-])[O-].[K+].[K+].[CH2:33](Br)[C:34]([C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1)=[O:35]>CN(C=O)C>[O:1]1[CH2:5][CH2:4][C:3]([C:6]2[C:7]([CH3:26])=[C:8]([CH:19]=[CH:20][C:21]=2[S:22]([CH3:25])(=[O:24])=[O:23])[C:9]([C:11]2[CH:12]=[N:13][N:14]([CH2:17][CH3:18])[C:15]=2[O:16][CH2:33][C:34]([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)=[O:35])=[O:10])=[N:2]1

참가 물질

5

반응물 3

HCID 6259Phenacyl bromideHCID 11430Potassium CarbonateHCID 178463114HCID 178463114, 화합물

생성물 1

HCID 154774574-[3-(4,5-Dihydroisoxazol-3-yl)-4-methylsulfonyl-2-methylbenzoyl]-1-ethyl-5-phenacyloxypyrazole수율 64.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

0.20 g of 4-[3-(4,5-dihydroisoxazol-3-yl)-4-methylsulfonyl-2-methylbenzoyl]-1-ethyl-5-hydroxypyrazole was dissolved in 10 ml of DMF, and 0.11 g of potassium carbonate, then 0.13 g of phenacyl bromide were added. The resulting solution was stirred at room temperature overnight. The reaction solution was poured into ice water, and extracted with ethyl acetate. The organic layer was washed 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 residue. The obtained crystals were separated by filtration to give 0.17 g of the title compound as white crystals. m.p. 177~179° C.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed 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 residue
  6. customThe obtained crystals were separated by filtration

출처 및 근거

ORD 기록
ord-abb9c3034bb7408e91264ea05b3bd8b6
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06147031

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