Water → HCID 20763143, compound

To a solution of [3-(2-Hydroxy-ethylamino)-propyl]-carbamic acid tert-butyl ester (900 mg, 4.1 mmol) in THF (20 mL) was added a 1M solution of BH3 in THF. The mixture was refluxed for 24 hours under nitrogen. The reaction was allowed to cool down and water (5 mL) was carefully added with vigorous stirring. The reaction mixture was concentrated to low volume and treated with a 6M aqueous solution of HCl (60 mL). The mixture was refluxed for 24 h. The mixture was concentrated to dryness then co-evaporated several time with methanol to give the desired 2-(3-methylamino-propylamino)-ethanol (399 mg, 2.46 mmol)

1. temperatureThe mixture was refluxed for 24 hours under nitrogen
2. temperatureto cool down
3. concentrationThe reaction mixture was concentrated to low volume
4. additiontreated with a 6M aqueous solution of HCl (60 mL)
5. temperatureThe mixture was refluxed for 24 h
6. concentrationThe mixture was concentrated to dryness

ORD record

ord-c8e44cb9376444d0b77131b8e01d1a40

Source dataset

uspto-grants-2012_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08202511B2