5-Bromopyrimidine → HCID 23119574、化合物
反応式
C([N:3]1[C:9]2[N:10]=[CH:11][C:12](C#C)=[CH:13][C:8]=2[C:7](=[O:16])[N:6](C)[C:5]2[CH:18]=[CH:19][CH:20]=[N:21][C:4]1=2)C.BrC1C=NC=NC=1>>[N:21]1[C:4]2[C:5](=[N:6][C:7](=[O:16])[C:8]3[CH:13]=[CH:12][CH:11]=[N:10][C:9]=3[N:3]=2)[CH:18]=[CH:19][CH:20]=1参加物
3
実験手順
By a procedure analogous to that described in Example 51b, 5,11-dihydro-11-ethyl-8-ethynyl-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (0.1 g, 0.36 mmol) was coupled with 5-bromopyrimidine (59 mg, 0.37 mmol) to give 65 mg of 5,11-Dihydro-11-ethyl-5-methyl-8-(5-pyrimidyl)ethynyl-(-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (65 mg). A mixture containing this coupled product (65 mg), cyclohexene (0.07 mL), and 10% palladium on carbon (60 mg) in 2 mL of ethanol was heated in a sealed tube at 95° C. for 5 hours. The reaction mixture was filtered through Celite and concentrated. Purification of the residue by flash chromatography, eluting with methanol/dichloromethane, and recrystallization from ethyl acetate/hexanes provided 27 mg of the title compound, m.p. 142°-143° C.
出典と根拠
- ORDレコード
- ord-dde71374fcc04796bc3fe6a40657542c