HRID2234977

反应详情

EQUATION

反应方程式

HRID 2234977 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 4-chloro-N-(2-chloro-4-pyridinyl)benzenesulfonamide (D3) (350 mg, 1 mmol), 5-methylfuran-2-boronic acid (150 mg, 1.2 mmol), sodium carbonate (230 mg, 2.2 mmol) and dichlorobis(triphenylphosphine) palladium(0) (20 mg, 15 mol %) in 1,2-dimethoxyethane (3 ml) and water (1 ml) was microwaved at 120° C. for 20 min. The reaction mixture was partitioned between ethyl acetate (5 ml) and water (5 ml) and the organic phase was dried and evaporated. Purification by column chromatography eluting with 5-50% ethyl acetate in hexanes afforded the title compound (D4), MS (ES+) m/e 349, 351 [M+H]+.

WORKUP

后处理

  1. customwas microwaved at 120° C. for 20 min
  2. customThe reaction mixture was partitioned between ethyl acetate (5 ml) and water (5 ml)
  3. customthe organic phase was dried
  4. customevaporated
  5. customPurification by column chromatography
  6. washeluting with 5-50% ethyl acetate in hexanes