반응 #51065

반응 방정식

4-chloro-6,7-dihydro-5H-cyclopenta[4,5]thieno[2,3-d]pyrimidine

diethylamine

diethylamine

t-butanol

EtOAc

→

desired product

N,N-diethyl-5,6,7,8-Tetrahydro[1]benzothieno[2,3-d]pyrimidin-4-amine

용매

H2O HCl

반응 조건

후처리

1. 1
   온도The mixture was heated
2. 2
   온도to reflux
3. 3
   온도heated
4. 4
   온도at reflux for an additional 1 h
5. 5
   기타reaction

실험 절차

To a slurry of 0.044 g 4-chloro-6,7-dihydro-5H-cyclopenta[4,5]thieno[2,3-d]pyrimidine (0.196 mmol) in 1 mL of 100:1 H2O/HCl was added 0.014 g (0.02 mL, 0.106 mmol) diethylamine. The mixture was heated to reflux, and an additional 0.2 mL diethylamine and 1 mL of t-butanol were added and heated continued at reflux for an additional 1 h. TLC (20% EtOAc/80% pet ether) showed complete reaction and the 1H NMR of the isolated material was consistent with the desired product.

출처