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Diethylamine → N,N-diethyl-2-nitrobenzenesulfonamide

HRID 1105747
ノート
印刷プレビュー

反応式

HRID 1105747 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8021DiethylamineHCID 155402-Nitrobenzenesulfonyl chlorideHCID 10197650Diethylammonium chloride

生成物 1

HCID 4229519N,N-diethyl-2-nitrobenzenesulfonamide収率 79.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a682d72d6d1d4929b32ac7cee12821b4
出典データセット
uspto-grants-1982_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04310346

反応ノート

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