Water → HCID 178426042、化合物
反応式
[O:1]1[CH2:5]CCC1.[CH3:6][C:7]1[N:12]=[C:11]([C:13]([NH2:15])=O)[CH:10]=[C:9]([C:16]([F:19])([F:18])[F:17])[CH:8]=1.C(N1C=CN=C1)([N:22]1C=CN=C1)=O.N12CCCN=C1CCCCC2.[OH2:43]>>[CH3:6][C:7]1[N:12]=[C:11]([C:13]2[NH:22][O:43][C:5](=[O:1])[N:15]=2)[CH:10]=[C:9]([C:16]([F:19])([F:18])[F:17])[CH:8]=1参加物
6
実験手順
To 3 ml of tetrahydrofuran were added 0.74 g of 6-methyl-4-trifluoromethylpyridine-2-carboxamide=oxime and 0.41 g of 1,1′-carbonyldiimidazole, and the mixture was stirred at room temperature for 1 hour and 30 minutes. Thereafter, 0.39 g of 1,8-diazabicyclo[5,4,0]undec-7-ene was added, and the mixture was stirred for 12 hours. To the reaction solution were added water and a 10% aqueous HCl solution, the resultant solution was extracted with ethyl acetate three times, and the organic layers were combined, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.6 g of 3-(6-methyl-4-trifluoromethylpyridin-2-yl)-1,2,4-oxadiazol-5-one (present compound (54)).
後処理
- stirringthe mixture was stirred for 12 hours
- extractiona 10% aqueous HCl solution, the resultant solution was extracted with ethyl acetate three times
- dry with materialdried with anhydrous magnesium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-d060f35d747a4d88b74e31ea397f088f
- 出典データセット
- uspto-grants-2012_11
- 特許番号
- US08318776B2
反応ノート
読み込み中…