反应详情

To a solution of 4-chloro-butyryl chloride (1.12 ml, 10.0 mmol) and dimethyl-amine hydrochloride (4.1 g, 50.0 mmol) in THF at 5° C. was added 2M NaOH (30 ml, 60.0 mmol) dropwise over 30 minutes while maintaining reaction temperature between 5-10° C. The reaction was stirred for additional 1.5 h and was concentrated, extracted with EtOAc (×2). The combined organic layer was washed with 1M HCl (×2), brine, dried over Na2SO4, and concentrated in vacuo to yield the title compound as colorless oil (1.5 g, ˜100%). The crude was used without further purification.

1. temperaturewhile maintaining
2. customreaction temperature between 5-10° C
3. concentrationwas concentrated
4. extractionextracted with EtOAc (×2)
5. washThe combined organic layer was washed with 1M HCl (×2), brine
6. dry with materialdried over Na2SO4
7. concentrationconcentrated in vacuo