N,N-Dimethylaniline → HCID 86664785、化合物
反応式
O[C:2]1[N:7]2[N:8]=[CH:9][CH:10]=[C:6]2[N:5]=[C:4]([CH:11]2[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:12]2)[CH:3]=1.CN(C)C1C=CC=CC=1.P(Cl)(Cl)([Cl:34])=O>>[Cl:34][C:2]1[N:7]2[N:8]=[CH:9][CH:10]=[C:6]2[N:5]=[C:4]([CH:11]2[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:12]2)[CH:3]=1参加物
4
反応条件
- 温度
- 50 °C
実験手順
To a mixture of tert-butyl 3-(7-hydroxypyrazolo[1,5-a]pyrimidin-5-yl)pyrrolidine-1-carboxylate (3.70 g, 12.0 mmol) and dimethylaniline (4.0 mL, 30 mml) was added phosphoryl trichloride (40 mL). The mixture was heated at 50° C. for 5 h and concentrated in vacuo. The residue was diluted with methylene chloride (100 mL) and quenched with saturated NaHCO3 (100 mL). The mixture was separated and the aqueous layer was extracted with chloride (100 mL×2). The combined organic layers were dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by Biotage (CH2Cl2/EtOAc, 20:1 to 4:1). LC/MS RT=2.09 min (5 min method). Mass calculated for, M+H 322.12, observed 337.14.