Acetic Acid → 2(3H)-Benzoxazolone, 5-[[2-[(4-fluoro-3-methoxy-5-methylphenyl)amino]-5-methyl-4-pyrimidinyl]amino]-3-[(phosphonooxy)methyl]-
반응식
[P:1]([O:13][CH2:14][N:15]1[C:19]2[CH:20]=[C:21]([NH:24][C:25]3[C:30]([CH3:31])=[CH:29][N:28]=[C:27]([NH:32][C:33]4[CH:38]=[C:37]([CH3:39])[C:36]([F:40])=[C:35]([O:41][CH3:42])[CH:34]=4)[N:26]=3)[CH:22]=[CH:23][C:18]=2[O:17][C:16]1=[O:43])([O:8]C(C)(C)C)([O:3]C(C)(C)C)=[O:2].CC(O)=O>O>[P:1]([OH:8])([OH:3])([O:13][CH2:14][N:15]1[C:19]2[CH:20]=[C:21]([NH:24][C:25]3[C:30]([CH3:31])=[CH:29][N:28]=[C:27]([NH:32][C:33]4[CH:38]=[C:37]([CH3:39])[C:36]([F:40])=[C:35]([O:41][CH3:42])[CH:34]=4)[N:26]=3)[CH:22]=[CH:23][C:18]=2[O:17][C:16]1=[O:43])=[O:2]참가 물질
4
반응 조건
- 온도
- 65 °C
실험 절차
To the crude di-tert-butyl (5-(2-(4-fluoro-3-methoxy-5-methylphenylamino)-5-methylpyrimidin-4-ylamino)-2-oxobenzo[d]oxazol-3(2H)-yl)methyl phosphate, was added HOAc (280 mL) and H2O (70 mL), the resultant light brown homogeneous solution was stirred at 65° C. (note: a lighter color ppt was formed between 15-45 min). The reaction was monitored by LC-MS. After 1 h, the mixture was cooled to rt, ppt was collected by filtration, washing with H2O (˜50 mL×2). Product (5-(2-(4-fluoro-3-methoxy-5-methylphenylamino)-5-methylpyrimidin-4-ylamino)-2-oxobenzo[d]oxazol-3(2H)-yl)methyl dihydrogen phosphate was obtained as a light pinkish beige color solid and was used directly in salt formation.