Hydrochloric Acid → 3-Chloro-3-ethyl-2-nitrosopentan-1-ol

2-Cyclohexylidene ethanol (VI) (23 g) was dissolved in glacial acetic acid (76 ml). Amyl nitrite (21.5 g) was added and the mixture was cooled in an ice-salt bath. The cooled solution was treated dropwise with cold concentrated hydrochloric acid (23 ml) with stirring. After the addition of the acid was complete the reaction mixture was stirred at the same temperature for 30 min, followed by cooling in an acetone-carbon dioxide bath for 10 min. The buff-coloured solid was filtered off, washed with cold methanol and recrystallised from acetone to give the nitrosochloride (V) (15 g; yield 43%) as colourless needles, m.p. 130°.

1. temperaturethe mixture was cooled in an ice-salt bath
2. additionAfter the addition of the acid
3. stirringwas stirred at the same temperature for 30 min
4. temperatureby cooling in an acetone-carbon dioxide bath for 10 min
5. filtrationThe buff-coloured solid was filtered off
6. washwashed with cold methanol
7. customrecrystallised from acetone

ORD-Eintrag

ord-3047003258824e88b21bac2f020dda5b

Quelldatensatz

uspto-grants-1976_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US03963719