4-[4-Chloro-5-(2-chloro-5-methoxy-phenoxy)-6-methyl-pyrimidin-2-yl]-morpholine → 4-tert-butyl-N-[5-(2-chloro-5-methoxy-phenoxy)-6-methyl-2-(morpholin-4-yl)-pyrimidin-4-yl]-benzenesulphonamide

HRID 37091

반응식

HRID 37091 반응식
Cl[C:2]1[C:7]([O:8][C:9]2[CH:14]=[C:13]([O:15][CH3:16])[CH:12]=[CH:11][C:10]=2[Cl:17])=[C:6]([CH3:18])[N:5]=[C:4]([N:19]2[CH2:24][CH2:23][O:22][CH2:21][CH2:20]2)[N:3]=1.[K].[C:26]([C:30]1[CH:35]=[CH:34][C:33]([S:36]([NH2:39])(=[O:38])=[O:37])=[CH:32][CH:31]=1)([CH3:29])([CH3:28])[CH3:27]>CS(C)=O>[C:26]([C:30]1[CH:35]=[CH:34][C:33]([S:36]([NH:39][C:2]2[C:7]([O:8][C:9]3[CH:14]=[C:13]([O:15][CH3:16])[CH:12]=[CH:11][C:10]=3[Cl:17])=[C:6]([CH3:18])[N:5]=[C:4]([N:19]3[CH2:24][CH2:23][O:22][CH2:21][CH2:20]3)[N:3]=2)(=[O:37])=[O:38])=[CH:32][CH:31]=1)([CH3:29])([CH3:27])[CH3:28]

참가 물질

4

반응물 2

HCID 189389104-[4-Chloro-5-(2-chloro-5-methoxy-phenoxy)-6-methyl-pyrimidin-2-yl]-morpholineHCID 66748434p-t-Butylbenzenesulfonamide potassium

생성물 1

HCID 199347354-tert-butyl-N-[5-(2-chloro-5-methoxy-phenoxy)-6-methyl-2-(morpholin-4-yl)-pyrimidin-4-yl]-benzenesulphonamide수율 93%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

10.7 g of 4-[4-chloro-5-(2-chloro-5-methoxy-phenoxy)-6-methyl-pyrimidin-2-yl]-morpholine and 21.6g of p-t-butyl-benzene sulphonamide potassium in 150 ml of dry dimethyl sulphoxide were heated to 120° C. under argon for 16 hours. Thereafter, the dimethylsulphoxide was distilled off, the residue was partitioned between ethyl acetate and 1N hydrochloric acid and the organic phase was washed neutral. The organic phase was dried, the solvent was evaporated and the residue was recrystallized from dichloromethane-ethanol. There were obtained 14.7 g 4-tert-butyl-N-[5-(2-chloro-5-methoxy-phenoxy)-6-methyl-2-(morpholin-4-yl)-pyrimidin-4-yl]-benzenesulphonamide, m.p 154° C., MS: M=546.

후처리

  1. distillationThereafter, the dimethylsulphoxide was distilled off
  2. customthe residue was partitioned between ethyl acetate and 1N hydrochloric acid
  3. washthe organic phase was washed neutral
  4. customThe organic phase was dried
  5. customthe solvent was evaporated
  6. customthe residue was recrystallized from dichloromethane-ethanol

출처 및 근거

ORD 기록
ord-dc856f450a234514a5ac03c174fae505
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05420129

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