HRID32638

反应详情

EQUATION

反应方程式

HRID 32638 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Boron tribromide (1.0M in DCM) (10.1 mL) was added dropwise to 6-[4-(4-methoxyphenyl)-1-methyl-1H-imidazol-5-yl]thieno[2,3-d]pyrimidin-4-amine (Intermediate 107) (0.91 g) in DCM (20 mL) then stirred for 5 days at ambient temperature. The reaction mixture was concentrated in vacuo and the residue partitioned between DCM and water. The aqueous layer was separated and extracted with DCM (3×20 mL), the aqueous layer was then adjusted to pH 9 with concentrated aqueous NH3, the resultant solid filtered and dried in vacuo to give the title compound as a brown solid (623 mg, 71%);

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customthe residue partitioned between DCM and water
  3. customThe aqueous layer was separated
  4. extractionextracted with DCM (3×20 mL)
  5. filtrationthe resultant solid filtered
  6. customdried in vacuo