Cysteamine Hydrochloride → HCID 19593910, compound

Temperature

75 °C

N-(2-Chloroethyl)-tetrahydropyran-2-ylthioacetamide (0.48 g, 2 mmol), 2-mercaptoethylamine hydrochloride (0.34 g, 3 mmol), potassium hydroxide (0.34 g, 6 mmol) methanol (5 cm3) and water (1 cm3) were mixed and heated at 75° C. for 2 h. After cooling, 111acetone (50 cm3) was added and the resulting mixture filtered. Volatile components were removed from the filtrate under reduced pressure to give a pale yellow residue. This material was purified firstly by chromatography on silica using a mixture of ethyl acetate, methanol, and aqueous ammonia (90:9:1) as the eluant and then by reverse phase h.p.l.c. using aqueous acetonitrile as the eluant. The purified N-[2-(2-aminoethylthio)ethyl]-tetrahydropyran-2-ylthioacetamide (1 g, 32%) was obtained as a pale yellow oil.

1. temperatureAfter cooling
2. filtrationthe resulting mixture filtered
3. customVolatile components were removed from the filtrate under reduced pressure
4. customto give a pale yellow residue
5. customThis material was purified firstly by chromatography on silica using
6. additiona mixture of ethyl acetate, methanol, and aqueous ammonia (90:9:1) as the eluant

ORD record

ord-0239555b9376414ba04bd0a03a007e4f

Source dataset

uspto-grants-1999_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05932707