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Hydrochloric Acid → HCID 2836736, 화합물

HRID 1012302
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HRID 1012302 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([S:8](Cl)(=[O:10])=[O:9])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].[C:15]([NH2:19])([CH3:18])([CH3:17])[CH3:16].Cl>C(Cl)(Cl)Cl>[C:15]([NH:19][S:8]([C:5]1[CH:6]=[CH:7][C:2]([CH3:1])=[C:3]([N+:12]([O-:14])=[O:13])[CH:4]=1)(=[O:10])=[O:9])([CH3:18])([CH3:17])[CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 6385Tert-ButylamineHCID 5606384-Methyl-3-nitrobenzenesulfonyl chloride

생성물 1

HCID 2836736HCID 2836736, 화합물수율 94.6%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a solution of 4-methyl-3-nitrobenzenesulfonyl chloride (5.40 g, 22.9 mmol) in chloroform (50 ml) was added tert-butylamine (6.00 ml, 57.1 mmol) under ice-cooling, and the mixture was stirred at room temperature for 2.5 hr. To the reaction mixture was added 1N hydrochloric acid, and the mixture was extracted with chloroform. The organic layer was successively washed with water, saturated aqueous sodium hydrogen carbonate solution and saturated brine, and dried over anhydrous sodium sulfate. After filtration, the solvent was evaporated under reduced pressure, and hexane was added to the residue. The precipitated solid was collected by filtration and dried in vacuo to give N-tert-butyl-4-methyl-3-nitrobenzenesulfonamide (5.89 g, yield 94.6%).

후처리

  1. temperaturecooling
  2. extractionthe mixture was extracted with chloroform
  3. washThe organic layer was successively washed with water, saturated aqueous sodium hydrogen carbonate solution and saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationAfter filtration
  6. customthe solvent was evaporated under reduced pressure, and hexane
  7. additionwas added to the residue
  8. filtrationThe precipitated solid was collected by filtration
  9. customdried in vacuo

출처 및 근거

ORD 기록
ord-0768500b70a1478b9785b10d729717e9
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07977331B1

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