HRID385808

反应详情

EQUATION

反应方程式

HRID 385808 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-(6-bromopyridin-2-yl)-2-hydroxyethanone (2.2 g, 10.18 mmol) in ethanol (127 mL) was charged with sodium borohydride (0.385 g, 10.18 mmol). After 30 minutes, the reaction was concentrated to dryness and then partitioned between ethyl acetate (50 mL) and 3:1 saturated aqueous sodium bicarbonate:water (25 mL). The layers were separated and the organic layer was washed with brine (25 mL), dried over sodium sulfate, filtered, and concentrated to afford the title compound. 1H NMR (600 MHz, DMSO): δ 7.69 (m, 1H), 7.46 (m, 2H), 5.50 (d, J=5.0 Hz, 1H), 4.69 (m, 1H), 4.49 (m, 1H), 3.61 (m, 1H), 3.46 (m, 1H).

WORKUP

后处理

  1. concentrationthe reaction was concentrated to dryness
  2. custompartitioned between ethyl acetate (50 mL) and 3:1 saturated aqueous sodium bicarbonate
  3. customThe layers were separated
  4. washthe organic layer was washed with brine (25 mL)
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated