Triethylamine → 2-Bromo-1-cyclohexyl-3-dimethylamino-propenone

Temperatur

0 °C

To an ice cold solution of 1.18 g (6.51 mmol) of 1-cyclohexyl-3-dimethylamino-propenone in 8 mL of dichloromethane was added dropwise 1.04 g (6.51 mmol) of bromine via an addition funnel. The reaction mixture was stirred at 0° C. for 0.5 h and then 0.9 mL (6.51 mmol) of triethylamine in 10 mL of ether was added dropwise. The mixture was stirred at 0° C. for 1 h and allowed to warm up to rt. A light yellow solid precipitated from the solution, and it was separated by filtration. The filtrate was then concentrated to give 1.69 g of 2-bromo-1-cyclohexyl-3-dimethylamino-propenone as a brown solid as indicated by 1H NMR. The product was used in the next reaction without any further purification.

1. stirringThe mixture was stirred at 0° C. for 1 h
2. temperatureto warm up to rt
3. customA light yellow solid precipitated from the solution, and it
4. customwas separated by filtration
5. concentrationThe filtrate was then concentrated

ORD-Eintrag

ord-8fe01bfc8ea44ddb88271c063a992a98

Quelldatensatz

uspto-grants-2007_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07196111B2