反应详情

温度

70 °C

To 4.16 g (16 mMol) of [4-(4-chloro-7H-pyrrolo[2,3-d]pyrimidin-6-yl)-phenyl]-methanol (see Step 108.3) and 1.99 g (16 mMol) of 2-methoxy-pyridin-4-ylamine [see Rec. Trav. Chim. (1955) 74, 1160; prepared from 2-methoxy-4-nitro-pyridine-1-oxide by hydrogenation in the presence of Raney-Nickel in methanol/THF] in 90 ml degassed DMF under N2-atmosphere, 996 mg of R(+)-BINAP [R(+)-2,2′-bis-(diphenylphosphino)-1,1′-binaphthalin); 1.6 mMol], 414 mg Pd2(dba)3.CHCl3 [tris(dibenzylideneacetone)dipalladium (0) chloroform complex; 0.40 mMol] and 3.08 g (32 mMol) of sodium-tert-butylate are subsequently added. The red solution is stirred at 70° C. over night and then poured into a mixture of 0.5 l of EtOAc and 1 l buffer (7.8 g of NaH2PO4.2H2O, 5 g of Na2HPO4.2H2O in 1 l H2O). After stirring for 1 h, the title compound is filtered off and washed with water and EtOAc; HPLC (conditions see Examples 67-78) tR=8.2 min; MS-ES+: (M+H)+=348.

1. customdegassed DMF under N2-atmosphere
2. stirringAfter stirring for 1 h
3. filtrationthe title compound is filtered off
4. washwashed with water and EtOAc