Ammonium Chloride → HCID 90389379、化合物
反応式
CC(C)([O-])C.[K+].Cl[CH2:8][CH:9]1[O:13][N:12]=[C:11]([CH:14]([F:16])[F:15])[CH2:10]1.[NH4+].[Cl-]>C1COCC1>[F:15][CH:14]([F:16])[C:11]1[CH:10]2[CH:9]([CH2:8]2)[O:13][N:12]=1参加物
5
実験手順
A solution of potassium tert-butoxide (1.0 M in THF, 66.3 mL, 66.3 mmol) was added dropwise to a solution of 5-(chloromethyl)-3-(difluoromethyl)-4,5-dihydroisoxazole (16a rac, 9.0 g, 53.1 mmol) in THF (70 mL) at 0° C. The reaction mixture was stirred for 30 min, then aqueous saturated NH4Cl solution was added slowly. The mixture was extracted with Et2O (2×), and the combined organic extracts were dried over MgSO4. The filtrate was concentrated under reduced pressure. The residue was purified by silica gel chromatography (0-60% Et2O/pentane gradient) to give the title compound as an oil (5.29 g, 75% yield)
後処理
- extractionThe mixture was extracted with Et2O (2×)
- dry with materialthe combined organic extracts were dried over MgSO4
- concentrationThe filtrate was concentrated under reduced pressure
- customThe residue was purified by silica gel chromatography (0-60% Et2O/pentane gradient)
出典と根拠
- ORDレコード
- ord-706c982f39a74463bfc177bb11c65822
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09085576B2
反応ノート
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