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Water → HCID 3591734, 화합물

HRID 1356614
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HRID 1356614 반응식
[H-].[Na+].[CH3:3][C:4]1[CH:20]=[CH:19][C:7]([NH:8][S:9]([C:12]2[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=2)(=[O:11])=[O:10])=[CH:6][C:5]=1[N+:21]([O-:23])=[O:22].S(OC)(O[CH3:28])(=O)=O.O>CN(C=O)C>[CH3:28][N:8]([S:9]([C:12]1[CH:13]=[CH:14][C:15]([CH3:18])=[CH:16][CH:17]=1)(=[O:11])=[O:10])[C:7]1[CH:19]=[CH:20][C:4]([CH3:3])=[C:5]([N+:21]([O-:23])=[O:22])[CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 6497Dimethyl SulfateHCID 24758Sodium hydrideHCID 27968454-methyl-N-(4-methyl-3-nitrophenyl)benzenesulfonamide

생성물 1

HCID 3591734HCID 3591734, 화합물수율 76%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a suspension of sodium hydride (60%, 0.14 g (3.50 mmol)) in DMF (3.0 ml), 4′-methyl-3′-nitro-p-toluenesulfonanilide (1.00 g (3.26 mmol)) was added with stirring at room temperature. To the resulting mixture, after 15 minutes' stirring at room temperature, dimethyl sulfate (0.34 ml (3.56 mmol)) was added dropwise. After one hours' stirring at room temperature, the reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed with water and saturated sodium chloride solution, successively, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. Diethyl ether was added to the residue, and the solid separated was filtered and washed to give 0.79 g (76%) of the title compound as pale yellow crystals.

후처리

  1. additionwas added
  2. stirringTo the resulting mixture, after 15 minutes' stirring at room temperature
  3. stirringAfter one hours' stirring at room temperature
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with water and saturated sodium chloride solution
  6. dry with materialsuccessively, dried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. additionDiethyl ether was added to the residue
  9. customthe solid separated
  10. filtrationwas filtered
  11. washwashed

출처 및 근거

ORD 기록
ord-641338928d4b4508b1d7dd5b96cf1999
출처 데이터셋
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06586617B1

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