反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:9][C:10]([F:13])([F:12])[F:11])=[CH:4][N:3]=1.C1C(=O)N([Br:21])C(=O)C1.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1.C(Cl)(Cl)(Cl)Cl>C(Cl)Cl>[Br:21][CH2:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:9][C:10]([F:11])([F:13])[F:12])=[CH:4][N:3]=1参加物
6
反応条件
- 温度
- 80 °C
実験手順
Add 2-methyl-5-(2,2,2-trifluoroethoxy)-pyridine (2.5 g, 13.1 mmol), NBS (2.3 g, 13.1 mmol) and benzoyl peroxide (50 mg) to a flask containing carbon tetrachloride (30 mL). Heat the mixture at 80° C. in a sealed flask for 16 h. Cool the flask, add NBS (1.1 g, 6.5 mmol) and benzoyl peroxide (100 mg), then continue heating at 80° C. for an additional 5 h. Cool the mixture, dilute with DCM, then wash with saturated sodium bisulfite (10 mL). Collect the organic layer and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (9:1) to obtain the desired intermediate (460 mg, 13%).
後処理
- temperatureCool the flask
- temperaturecontinue heating at 80° C. for an additional 5 h
- temperatureCool the mixture
- washwash with saturated sodium bisulfite (10 mL)
- customCollect the organic layer
- concentrationconcentrate in vacuo
- customPurify by chromatography on silica gel eluting with hexane/EtOAc (9:1)
出典と根拠
- ORDレコード
- ord-e1def4c742d748bc8e65026f28389864
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08022062B2
関連ノート
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