HRID84436

反应详情

EQUATION

反应方程式

HRID 84436 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6,7-Dihydropyrido[3,2-b]thieno[2,3-d]oxepin-9-yl-(2-chlorophenyl)-2-bromoethanone from Example 37 (65.0 mg, 0.150 mmol) was suspended in formamide (2 mL, 50 mmol). The reaction was microwaved on 300 watts at 130° C. for 20 minutes. Water was added and the product was extracted with ethylacetate. The organic layer was washed with water twice and brine, dried over MgSO4, and evaporated to dryness. The crude product was purified on silica gel column, eluting with 25% of ethylacetate in hexane to give 129 (yield 10 mg, 18%). MS (ESI+) 381.1

WORKUP

后处理

  1. customThe reaction was microwaved on 300 watts at 130° C. for 20 minutes
  2. extractionthe product was extracted with ethylacetate
  3. washThe organic layer was washed with water twice
  4. dry with materialbrine, dried over MgSO4
  5. customevaporated to dryness
  6. customThe crude product was purified on silica gel column
  7. washeluting with 25% of ethylacetate in hexane