Water → 3-(Azidomethyl)-5-(trifluoromethyl)isoxazole
反応式
CS(O[CH2:6][C:7]1[CH:11]=[C:10]([C:12]([F:15])([F:14])[F:13])[O:9][N:8]=1)(=O)=O.[N-:16]=[N+:17]=[N-:18].[Na+].O>CN(C=O)C>[N:16]([CH2:6][C:7]1[CH:11]=[C:10]([C:12]([F:15])([F:14])[F:13])[O:9][N:8]=1)=[N+:17]=[N-:18]参加物
5
実験手順
To a solution of 8.7 g (5-(trifluoromethyl)isoxazol-3-yl)methyl methanesulfonate in 87 mL DMF was added 9.23 g sodium azide. The reaction mixture was stirred 3 h at RT. 80 mL water was added under cooling. The mixture was extracted with diethyl ether (3×100 mL) and the organic layers were washed with water (3×100 mL) and then with sat. NaCl solution (1×100 mL). The combined organic layer was dried over Na2SO4, filtered off and concentrated in vacuo to yield 6.26 g of the title compound as a brown oil.
後処理
- temperatureunder cooling
- extractionThe mixture was extracted with diethyl ether (3×100 mL)
- washthe organic layers were washed with water (3×100 mL)
- dry with materialThe combined organic layer was dried over Na2SO4
- filtrationfiltered off
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-922f1767935b4225a5d543e9285cf157
- 出典データセット
- uspto-grants-2014_05
- 特許番号
- US08729105B2
反応ノート
読み込み中…