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Diethylamine → N,N-diethyl-2-nitrobenzenesulfonamide

HRID 1105747
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HRID 1105747 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[S:10](Cl)(=[O:12])=[O:11])([O-:3])=[O:2].[CH2:14]([NH:16][CH2:17][CH3:18])[CH3:15].Cl.C(NCC)C>O1CCCC1>[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[S:10]([N:16]([CH2:17][CH3:18])[CH2:14][CH3:15])(=[O:12])=[O:11])([O-:3])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8021DiethylamineHCID 155402-Nitrobenzenesulfonyl chlorideHCID 10197650Diethylammonium chloride

생성물 1

HCID 4229519N,N-diethyl-2-nitrobenzenesulfonamide수율 79.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 132.6 g of o-nitrobenzenesulfonyl chloride in 700 ml of tetrahydrofuran was added 88.5 g of diethylamine at 5°-15°. The reaction mixture was stirred at room temperature for 1 hour before the precipitated diethylamine hydrochloride was removed by filtration. The filtrate was evaporated to dryness in-vacuo and the residue dissolved in 1-chlorobutane. The 1-chlorobutane solution was washed with water, dried over magnesium sulfate and evaporated in-vacuo to give 122.4 g of o-nitro-N,N-diethylbenzenesulfonamide as a dark oil.

후처리

  1. customwas removed by filtration
  2. customThe filtrate was evaporated to dryness in-vacuo
  3. dissolutionthe residue dissolved in 1-chlorobutane
  4. washThe 1-chlorobutane solution was washed with water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated in-vacuo

출처 및 근거

ORD 기록
ord-a682d72d6d1d4929b32ac7cee12821b4
출처 데이터셋
uspto-grants-1982_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04310346

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