反应详情

温度

50 °C

Under a argon atmosphere, 29.0 g (128 mmol) of 4-chloro-6-ethoxy-carbonyl-7H-pyrrolo[2,3-d]pyrimidine and 18.0 ml (171 mmol) of 3-chloroaniline in 430 ml of n-butanol are stirred at 100° C. for 3 h (almost dissolved after≈1 h, then a thick suspension is formed). 400 ml of isopropanol/hexane (1:1) are then added to the reaction mixture cooled to≈50° C., and the product is filtered off and washed with isopropanol and hexane. Stirring in diethyl ether yields 4-(3-chloroanilino)-6-ethoxy-carbonyl-7H-pyrrolo[2,3-d]pyrimidine; 1H-NMR (DMSO-d6) 13.0 and 10.53 (2 sb, 2HN), 8.48 (s, 1H), 8.13 (m, 1H), 7.78 (dm, J=8, 1H), 7.76 (s, 1H), 7.45 (t, J=8, 1H), 7.21 (dm, J=8), 1H), 4.37 (q, J=7, 2H), 1.37 (t, J=7, 3H).

1. dissolutionalmost dissolved after≈1 h
2. customa thick suspension is formed)
3. filtrationthe product is filtered off
4. washwashed with isopropanol and hexane