HRID1408434

反应详情

EQUATION

反应方程式

HRID 1408434 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methyl N-[[2-chloro-5-(1-spiro[2H-1-benzopyran-3(4H), 2′-[1,3]dioxolan]-6-yl-1H-pyrazol-3-yl)phenyl]methyl]carbamate (i.e. the product of Example 9, Step B) (150 mg, 0.32 mmol) in acetone (15 mL) was added 3N HCl (4.5 mL). The reaction mixture was heated at 85° C. for 16 hrs when TLC analysis (50% ethyl acetate/pet ether) showed completion of reaction. The reaction mixture was cooled and the solvent was concentrated under vacuum. The resultant residue was partitioned between water and ethyl acetate. The organic phase was washed with water, brine, dried over Na2SO4 and concentrated under vacuum to give the title compound, a compound of the present invention, (90 mg, 68% yield) as a solid.

WORKUP

后处理

  1. customcompletion of reaction
  2. temperatureThe reaction mixture was cooled
  3. concentrationthe solvent was concentrated under vacuum
  4. customThe resultant residue was partitioned between water and ethyl acetate
  5. washThe organic phase was washed with water, brine
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated under vacuum