Dimethyl Sulfoxide → HCID 22241385、化合物

反応式

C(Cl)(=O)C(Cl)=O.CS(C)=O.[OH:11][CH2:12][C:13]1[C:40]([CH3:41])=[CH:39][CH:38]=[CH:37][C:14]=1[CH2:15][O:16][C:17]1[CH:18]=[C:19]([CH:34]=[CH:35][CH:36]=1)[O:20][CH2:21][C:22]1[N:31]([CH3:32])[C:30](=[O:33])[C:29]2[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=2)[N:23]=1.C(N(CC)CC)C>ClCCl>[CH3:41][C:40]1[CH:39]=[CH:38][CH:37]=[C:14]([CH2:15][O:16][C:17]2[CH:36]=[CH:35][CH:34]=[C:19]([O:20][CH2:21][C:22]3[N:31]([CH3:32])[C:30](=[O:33])[C:29]4[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=4)[N:23]=3)[CH:18]=2)[C:13]=1[CH:12]=[O:11]

参加物

実験手順

To a cooled (−78° C.) solution of oxalyl chloride (2.5 mL, 1.75 M in CH2Cl2) is added, dropwise, DMSO (80 mL). On complete addition, a solution of 2-[3-(2-hydroxymethyl-3-methyl-1 benzyloxy)-phenoxymethyl]-3-methyl-3H-quinazolin-4-one (120 mg, 0.28 mmol, example 101) in dichloromethane (1 mL) is added dropwise. This solution is stirred for 5 min then triethylamine (276 mL, 2 mmol) is added in one portion. The cold bath is removed and stirring continued for 10 min. The mixture is then diluted with ethyl acetate, washed with water and brine, dried over MgSO4 and concentrated to give the title compound as a solid. MS (ESI) 415 (M+H)+.