Sodium hydride → 4-tert-butyl-N-(6-chloropyrimidin-4-yl)benzenesulfonamide

HRID 2307

반응식

HRID 2307 반응식
[Cl:1][C:2]1[CH:7]=[C:6](Cl)[N:5]=[CH:4][N:3]=1.[C:9]([C:13]1[CH:18]=[CH:17][C:16]([S:19]([NH2:22])(=[O:21])=[O:20])=[CH:15][CH:14]=1)([CH3:12])([CH3:11])[CH3:10].[H-].[Na+]>CN(C)C=O.Cl.O>[C:9]([C:13]1[CH:18]=[CH:17][C:16]([S:19]([NH:22][C:6]2[CH:7]=[C:2]([Cl:1])[N:3]=[CH:4][N:5]=2)(=[O:20])=[O:21])=[CH:15][CH:14]=1)([CH3:12])([CH3:10])[CH3:11]

참가 물질

7

반응물 3

HCID 24758Sodium hydrideHCID 709434,6-DichloropyrimidineHCID 2228724-tert-Butylbenzenesulfonamide

생성물 1

HCID 108710784-tert-butyl-N-(6-chloropyrimidin-4-yl)benzenesulfonamide수율 69.4%

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

To a solution of 4,6-dichloropyrimidine (1.33 g) and 4-tert-butylbenzenesulfonamide (1.96 g) in dimethylformamide (20 ml) is added sodium hydride (60% dispersion-type, 714 mg). The mixture is stirred at room temperature for two hours, and the reaction solution is diluted with 10% hydrochloric acid and water. The mixture is extracted with ethyl acetate, and the ethyl acetate layer is washed, dried, and evaporated to remove the solvent. The residue is recrystallized from ethyl acetate to give 4-tert-butyl-N-(6-chloropyrimidin-4-yl)benzenesulfonamide (2.02 g).

후처리

  1. extractionThe mixture is extracted with ethyl acetate
  2. washthe ethyl acetate layer is washed
  3. customdried
  4. customevaporated
  5. customto remove the solvent
  6. customThe residue is recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-6c62f99d0fed4032b2e1262e33a10198
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728706

연결된 노트

불러오는 중…