反应详情

A solution of 246 mg (1.0 mMol) of 5-(6-chloro-pyrimidin-4-yloxy)-1H-indole (WO 03/099771; Stage 163.1) in 5.5 ml acetic acid is cooled to 10-15° C. Then 314 mg (5 mMol) NaBH3CN are added portionwise. After 1 h stirring, 9 g of ice are added and the mixture is concentrated partially in vacuo. The residue is dissolved in 25 ml 1 N NaOH and extracted three times with EtOAc. The organic layers are washed twice with water and brine, dried (Na2SO4) and concentrated at rt in vacuo: MS: [M+1]+=248; TLC(EtOAc/hexane 1:1): Rf=0.31.

1. concentrationthe mixture is concentrated partially in vacuo
2. dissolutionThe residue is dissolved in 25 ml 1 N NaOH
3. extractionextracted three times with EtOAc
4. washThe organic layers are washed twice with water and brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated at rt in vacuo