5,7-Dichloro-6-(2,6-difluorophenyl)pyrazolo[1,5-a]pyrimidine-3-carboxylic acid methyl ester → 5-Chloro-6-(2,6-difluorophenyl)pyrazolo[1,5-a]pyrimidine-3-carboxylic acid methyl ester
反応式
[CH3:1][O:2][C:3]([C:5]1[CH:6]=[N:7][N:8]2[C:13](Cl)=[C:12]([C:15]3[C:20]([F:21])=[CH:19][CH:18]=[CH:17][C:16]=3[F:22])[C:11]([Cl:23])=[N:10][C:9]=12)=[O:4]>C(O)C.O.C1COCC1.[Zn]>[CH3:1][O:2][C:3]([C:5]1[CH:6]=[N:7][N:8]2[CH:13]=[C:12]([C:15]3[C:20]([F:21])=[CH:19][CH:18]=[CH:17][C:16]=3[F:22])[C:11]([Cl:23])=[N:10][C:9]=12)=[O:4]参加物
6
実験手順
5 g (13.96 mmol) 5,7-Dichloro-6-(2,6-difluorophenyl)pyrazolo[1,5-a]pyrimidine-3-carboxylic acid methyl ester are dissolved in a mixture of 355 mL ethanol, 253 mL water and 136 mL THF. After addition of 5.8 g (89 mmol) zinc in portions, the mixture is vigorously stirred at rt for three hours. Stirring is continued over night. The reaction mixture is filtered via a glass microfibre filter and washed with plenty of ethanol. The solvent has been removed and the residue redissolved in ethyl acetate. After washing twice with brine and drying over Na2SO4, the solvent is evaporated and the residue is used in the next step as the crude contaminated product (2.3 g=51%).
後処理
- stirringStirring
- waitis continued over night
- filtrationThe reaction mixture is filtered via a glass microfibre
- filtrationfilter
- washwashed with plenty of ethanol
- customThe solvent has been removed
- dissolutionthe residue redissolved in ethyl acetate
- washAfter washing twice with brine
- dry with materialdrying over Na2SO4
- customthe solvent is evaporated
出典と根拠
- ORDレコード
- ord-b3c6a6e76e3949e0b68edd5ca03c071c
- 出典データセット
- uspto-grants-2015_02
- 特許番号
- US08957064B2
反応ノート
読み込み中…