HRID1976092

反应详情

EQUATION

反应方程式

HRID 1976092 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

At 0° C. to 1.0 g (6.24 mmol) of 1,3-naphthalenediol in tetrahydrofuran (20 mL) containing 1.5 mL of 2,6-lutidine was added 1.35 g (6.40 mmol) of 2-chlorobenzenesulfonyl chloride. The reaction mixture was stirred to ambient temperature overnight, quenched with 3 N hydrochloric acid, extracted into methylene chloride, and dried (MgSO4). Purification by flash chromatography (2% ethyl acetate/methylene chloride) gave 277 mg (13% yield) of the title compound as a colorless solid. 1H-NMR (300 MHz, DMSO-d6) δ 10.75 (s, 1 H), 8.06 (d, 1 H, J=1.7 Hz), 7.78-7.95 (m, 4 H), 7.43-7.57 (m, 3 H), 7.11 (d, 1 H, J=2 Hz), and 6.63 (d, 1 H, J=2 Hz).

WORKUP

后处理

  1. customquenched with 3 N hydrochloric acid
  2. extractionextracted into methylene chloride
  3. dry with materialdried (MgSO4)
  4. customPurification by flash chromatography (2% ethyl acetate/methylene chloride)