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

HRID 1082303

반응식

HRID 1082303 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-tertbutylbenzenesulfonamide (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-31127bca4c4c420e81a16e253c1c48ea
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05589478

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