Hydrochloric Acid → 2-(2,3-Dihydro-1,4-benzodioxin-2-yl)ethanamine

The 2-cyanomethyl-(2,3 dihydrobenzo[1,4]dioxine) was dissolved in THF (50 mL) and 1M BH3 in THF (80 mL, 80 mmol) was added and the reaction mixture refluxed for 5 h, then stirred at ambient temperature for 16 h. With ice bath cooling, 2N HCl was added until pH=1.0 was achieved. The reaction mixture was then stirred for 1 h at room temperature and evaporated in vacuo to yield an oil. The oil was partitioned between 3N NaOH and diethyl ether, and the diethyl ether solution was washed with brine, dried (Na2SO4) and evaporated in vacuo to yield crude 2-(2,3 dihydrobenzo[1,4]dioxin-2-yl)ethylamine.

1. temperaturethe reaction mixture refluxed for 5 h
2. temperatureWith ice bath cooling
3. stirringThe reaction mixture was then stirred for 1 h at room temperature
4. customevaporated in vacuo
5. customto yield an oil
6. customThe oil was partitioned between 3N NaOH and diethyl ether
7. washthe diethyl ether solution was washed with brine
8. dry with materialdried (Na2SO4)
9. customevaporated in vacuo

ORDレコード

ord-23779fdc1e0c43079946be52b228c655

出典データセット

uspto-grants-2013_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08497298B2