HRID253297

反应详情

EQUATION

反应方程式

HRID 253297 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of methyl 7-fluoro-2,3-dihydro-1,4-benzodioxine-5-carboxylate (400 mg, 1.88 mmol) in tetrahydrofuran (20 mL) was cooled to 0° C. and then added lithium aluminum hydride (3.78 mL, 1.0 M solution in tetrahydrofuran). The reaction mixture was allowed to warm to room temperature and stirred for 45 min, at which time water (143 μL) was added followed by 15% sodium hydroxide (143 μL) and then water (286 μL) again. The white precipitate was filtered and the filtrate was concentrated to give 345 mg (100%) of (7-fluoro-2,3-dihydro-1,4-benzodioxine-5-yl)methanol as a colorless oil: 1H NMR (400 MHz, CDCl3): 6.63 (dd, J=2.8, 8.8 Hz, 1H), 6.56 (dd, J=3.2, 9.2 Hz, 1H), 4.64 (d, J=6.4 Hz, 2H), 4.28-4.25 (m, 4H).

WORKUP

后处理

  1. additionwas added
  2. filtrationThe white precipitate was filtered
  3. concentrationthe filtrate was concentrated