Sodium Carbonate → 2-(3-Methoxy-4-methylsulfinylphenyl)-4-(3,4-dihydrocarbostyril-6-yl)thiazole

HRID 1489242노트

반응식

HRID 1489242 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[S:12][CH:13]=[C:14]([C:16]3[CH:17]=[C:18]4[C:23](=[CH:24][CH:25]=3)[NH:22][C:21](=[O:26])[CH2:20][CH2:19]4)[N:15]=2)[CH:6]=[CH:7][C:8]=1[S:9][CH3:10].C(=O)([O-])[O-:28].[Na+].[Na+]>C(Cl)(Cl)Cl.C(O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[S:12][CH:13]=[C:14]([C:16]3[CH:17]=[C:18]4[C:23](=[CH:24][CH:25]=3)[NH:22][C:21](=[O:26])[CH2:20][CH2:19]4)[N:15]=2)[CH:6]=[CH:7][C:8]=1[S:9]([CH3:10])=[O:28]

참가 물질

4

반응물 2

HCID 10340Sodium CarbonateHCID 100227982-(3-Methoxy-4-methylthiophenyl)-4-(3,4-dihydrocarbostyril-6-yl)thiazole

생성물 1

HCID 117415922-(3-Methoxy-4-methylsulfinylphenyl)-4-(3,4-dihydrocarbostyril-6-yl)thiazole

시약·촉매·용매 1

HCID 21889567Chloroform ethanol용매

실험 절차

In 150 ml of chloroform-ethanol was suspended 3.40 g of 2-(3-methoxy-4-methylthiophenyl)-4-(3,4-dihydrocarbostyril-6-yl)thiazole. Thereto was added, in small portions, 1.97 g of methachloroperbenzoic acid (80%) under ice-cooling. The mixture was stirred for 1 hour. Then, the mixture was returned to room temperature and stirred overnight. Thereto was added an aqueous sodium carbonate solution. The mixture was extracted with chloroform three times. The combined extract was washed with a saturated aqueous sodium chloride solution and dried over magnesium sulfate. The solvent was distilled off and the resulting crystals were recrystallized from dimethylformamide to obtain 0.50 g of 2-(3-methoxy-4-methylsulfinylphenyl)-4-(3,4-dihydrocarbostyril-6-yl)thiazole as light yellow acicular crystals.

후처리

  1. temperaturecooling
  2. customwas returned to room temperature
  3. stirringstirred overnight
  4. extractionThe mixture was extracted with chloroform three times
  5. extractionThe combined extract
  6. washwas washed with a saturated aqueous sodium chloride solution
  7. dry with materialdried over magnesium sulfate
  8. distillationThe solvent was distilled off
  9. customthe resulting crystals were recrystallized from dimethylformamide

출처 및 근거

ORD 기록
ord-912f68226f664a6aa114712fe5d8cd30
출처 데이터셋
uspto-grants-1997_10
특허 번호
US05677319

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