HRID2096700

反应详情

EQUATION

反应方程式

HRID 2096700 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Imidazole (2.27 g, 33.3 mmol) was added to a stirred solution of 2-hydroxymethyl-6-(1-hydroxy-1-methylethyl)pyridine (5.30 g, 31.7 mmol) and tert-butyldimethylsilylchloride (5.02 g, 33.3 mmol) in DMF (70 mL) and the mixture was stirred for 16 h at room temperature. The mixture was poured onto water, extracted with EtOAc, the organic portion was separated, dried (MgSO4), filtered and evaporated to give the title compound (8.19 g, 92%) as a colourless oil; NMR δH (400 MHz, CDCl3) 7.74-7.70 (1H, m), 7.40-7.38 (1H, m), 7.20-7.18 (1H, m), 5.34 (1H, s), 4.83 (2H, s), 1.52 (6H, s), 0.97 (9H, s), 0.13 (6H, s); (M+H)+ 282.

WORKUP

后处理

  1. additionThe mixture was poured onto water
  2. extractionextracted with EtOAc
  3. customthe organic portion was separated
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customevaporated