반응 #1471511

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1-(2,2-Diphenyl-benzo(1,3)dioxol-5-yl)-propan-1-one

bromine

→

2-bromo-1-(2,2-diphenyl-benzo(1,3)dioxol-5-yl)-propan-1-one

수율 96.0%

용매

carbon tetrachloride

반응 조건

후처리

1. 1
   추출it was extracted with saturated aqueous bicarbonate solution
2. 2
   세척The organic phase was washed with water and brine
3. 3
   건조dried over magnesium sulfate
4. 4
   농축concentrated

실험 절차

1-(2,2-Diphenyl-benzo(1,3)dioxol-5-yl)-propan-1-one (the compound of Preparation 42, 4.70 g, 14.23 mmol) was dissolved in carbon tetrachloride (60 mL) and bromine (0.74 mL, 14.36 mmol in 10 mL of carbon tetrachloride) was added dropwise. The reaction was stirred at ambient temperature 30 min and then it was extracted with saturated aqueous bicarbonate solution. The organic phase was washed with water and brine, dried over magnesium sulfate, and concentrated to afford 5.58 g (96%) of 2-bromo-1-(2,2-diphenyl-benzo(1,3)dioxol-5-yl)-propan-1-one as a dark orange oil which had: NMR δ7.68-7.37 (m, 12 H), 6.95 (d, J=8.3 Hz, 1 H), 5.21 (q, J=6.7 Hz, 1 H), 1.88 (d, J=6.6 Hz, 3 H).

출처