Triethylamine → HCID 57519920, Verbindung

Temperatur

0 °C

366 mg of bis(trichloromethyl)carbonate (1.234 mmol) were dissolved in 7 ml of DCM and cooled to 0° C. To this mixture the solution of 400 mg of 6-(trifluoromethyl)pyridin-2-amine (2.467 mmol) and 379 μl of triethylamine (5.43 mmol) in 9.7 ml DCM was slowly added over 60 minutes at 0° C., and stirring was continued for an additional 60 minutes at room temperature. 550 mg of 6-bromoquinolin-4-amine (2.467 mmol) and 379 μl of triethylamine (5.43 mmol) were suspended in 9.7 ml and subsequently slowly added to the reaction mixture at RT, which became a clear solution after 45 minutes. After stirring over night the reaction mixture was poured into ice water and stirred for 2 h. The precipitation formed was filtered off and dried in vacuum for 24 h. 810 mg of the desired product were obtained as an off white powder (yield: 80%). The quite pure raw material was used without further purification in the next step.

1. additionsubsequently slowly added to the reaction mixture at RT
2. customafter 45 minutes
3. stirringAfter stirring over night the reaction mixture
4. stirringstirred for 2 h
5. customThe precipitation
6. customformed
7. filtrationwas filtered off
8. customdried in vacuum for 24 h

ORD-Eintrag

ord-75cbc8e726af4a1ca4d5fc7b3a9538d9

Quelldatensatz

uspto-grants-2015_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09090592B2