反应详情

A solution of trans-4-(5-methyl-isoxazol-3-yl)-cyclohexanecarboxylic acid methyl ester (250 mg, 1.12 mmol) and N-chlorosuccinimide (164 mg, 1.23 mmol) in N,N-dimethylformamide (2.2 ml) was stirred for 24 h at room temperature. The reaction mixture was partitioned between tert-butyl methyl ether (50 ml) and water (50 ml). The layers were separated. The aqueous layer was extracted with one 50 ml-portion of tert-butyl methyl ether. The combined organic layers were washed with one 50 ml-portion of 0.1 M aqueous sodium hydroxide solution, one 50 ml-portion of water and one 30 ml-portion of brine, dried over anhydrous sodium sulfate and concentrated in vacuo to give the crude title compound (275 mg, 95%) as light yellow oil, which was used in the next step without further purification. MS m/e: 257 (M+)

1. customThe reaction mixture was partitioned between tert-butyl methyl ether (50 ml) and water (50 ml)
2. customThe layers were separated
3. extractionThe aqueous layer was extracted with one 50 ml-portion of tert-butyl methyl ether
4. washThe combined organic layers were washed with one 50 ml-portion of 0.1 M aqueous sodium hydroxide solution, one 50 ml-portion of water and one 30 ml-portion of brine
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated in vacuo