反応式
[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]1参加物
5
実験手順
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.
後処理
- extractionextracted with ethyl acetate
- washThe organic layer was washed with water
- dry with materialwith a saturated sodium chloride solution, and dried over anhydrous magnesium sulfate
- distillationThe solvent was distilled out under reduced pressure
- additionMethanol was added to the residue
- customThe obtained crystals were separated by filtration
出典と根拠
- ORDレコード
- ord-abb9c3034bb7408e91264ea05b3bd8b6
- 出典データセット
- uspto-grants-2000_11
- 特許番号
- US06147031
関連ノート
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