氢氧化钾 → 5-Bromo-3,3-dimethyl-1,2,3,4-tetrahydroisoquinoline

To a solution of Intermediate 24E (4.6 g) in ethylene glycol (50 mL) was added 50% aqueous KOH solution (23 mL) and the reaction was heated at 150° C. for 3 days. The reaction mixture was cooled, diluted with H2O, extracted with EtOAc twice. The combined organics were extracted with 1.5 N HCl solution, the aqueous layer was basified with 10% NaOH solution, extracted with EtOAc twice and the combined organics were washed with H2O, brine, dried over Na2SO4, filtered and concentrated to give Intermediate 24 (1.5 g, 39.4%) as a brown liquid. MS (ESI) m/z: 242.2 (M+H)+.

1. temperatureThe reaction mixture was cooled
2. extractionextracted with EtOAc twice
3. extractionThe combined organics were extracted with 1.5 N HCl solution
4. extractionextracted with EtOAc twice
5. washthe combined organics were washed with H2O, brine
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated

ORD记录

ord-01f7f50f506d4f88ab4124cd93c13b33

来源数据集

uspto-grants-2015_11

DOI

10.6084/m9.figshare.5104873.v1

专利号

US09192607B2