反応 #645317

反応方程式

1-(2-bromo-4-fluoro-phenyl)-butane-1,4-diol

→

title compound

収率 77.3%

2-(2-Bromo-4-fluoro-phenyl)-tetrahydro-furan

収率 77.3%

溶媒

1,2-dichloroethane

chloroform IPA

反応条件

後処理

1. 1
   その他Seal the tube
2. 2
   洗浄Wash the organic phase with aqueous saturated sodium chloride and water
3. 3
   乾燥Dry the mixture over sodium sulfate
4. 4
   濃縮Concentrate the solution in vacuo
5. 5
   その他Purify by column chromatography (20% ethyl acetate in hexane)

実験手順

Combine 1-(2-bromo-4-fluoro-phenyl)-butane-1,4-diol (1 g, 3.8 mmol), silver (I)hexafluoroantimonate (131 mg, 0.4 mmol), platinum(II) chloride (40 mg, 0.2 mmol) in 1,2-dichloroethane (10 mL) in a pressure tube. Seal the tube and heat the mixture overnight at 110° C. Dilute the mixture with chloroform-IPA (3:1, 100 mL). Wash the organic phase with aqueous saturated sodium chloride and water. Dry the mixture over sodium sulfate. Concentrate the solution in vacuo. Purify by column chromatography (20% ethyl acetate in hexane) to give the title compound as a pale yellow oil (0.72 g, 77%).

出典