Hydrochloric Acid → HCID 69885127, compound

The process is performed as in Example 2, starting with 5.8 g of N-[(1S)-2-hydroxy-1-(3-nitrobenzyl)ethyl]acetamide in 60 cm3 of aqueous 6N hydrochloric acid, for 10 hours at a temperature in the region of 100° C. After cooling the medium, the precipitate is filtered off and then washed with 30 cm3 of acetone and 3 times 50 cm3 of ether, and dried in an oven under reduced pressure (10 Pa) at a temperature in the region of 60° C. The filtrate is concentrated under reduced pressure (5 kPa) at about 5° C. The residue obtained is taken up in 30 cm3 of diethyl ether and the crystals are filtered off, washed with twice 30 cm3 of ether and dried in an oven under the same conditions as above. The 2 crops crystallized are combined. 5.65 g of (2S)-2-amino-3-(3-nitrophenyl)-1-propanol hydrochloride are obtained in the form of a beige-colored solid melting at 188° C.

1. temperatureAfter cooling the medium
2. filtrationthe precipitate is filtered off
3. washwashed with 30 cm3 of acetone and 3 times 50 cm3 of ether
4. customdried in an oven under reduced pressure (10 Pa) at a temperature in the region of 60° C
5. concentrationThe filtrate is concentrated under reduced pressure (5 kPa) at about 5° C
6. customThe residue obtained
7. filtrationthe crystals are filtered off
8. washwashed with twice 30 cm3 of ether
9. customdried in an oven under the same conditions as above
10. customThe 2 crops crystallized

ORD record

ord-b7a5cf76cc1343aca031818f0be9db9c

Source dataset

uspto-grants-2002_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06451821B1