Water → N-(2-Benzoyloxyethyl)pyridinium m-Nitrobenzenesulfonate

HRID 1614299

反応式

HRID 1614299 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([S:10]([O-:13])(=[O:12])=[O:11])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].[Na+].O.[Br-].[C:17]([O:25][CH2:26][CH2:27][N+:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)(=[O:24])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>C(Cl)Cl>[N+:1]([C:4]1[CH:5]=[C:6]([S:10]([O-:13])(=[O:11])=[O:12])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].[C:17]([O:25][CH2:26][CH2:27][N+:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)(=[O:24])[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1

参加物

5

反応物 3

HCID 962Water2 回HCID 31389Sodium 3-nitrobenzenesulfonateHCID 19762119N-(2-benzoyloxyethyl)pyridinium bromide

生成物 1

HCID 19762115N-(2-Benzoyloxyethyl)pyridinium m-Nitrobenzenesulfonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 11.26 grams (0.05 mol) of sodium m-nitrobenzenesulfonate in 50 milliters of water was added to a solution of 15.41 grams (0.05 mole) of N-(2-benzoyloxyethyl)pyridinium bromide, prepared as described in Example 2, in 50 milliters of water. The resultant solution was treated with methylene chloride resulting in the formation of three layers. The center layer was isolated, treated with ligroine (bp=70°-90° C.) and allowed to stand with spatula scratching of the oil. Crystallization occurred and the solid was collected, washed with ether and recrystallized from acetonitrile. The yield of product was 6.6 grams (30.67% of theory); mp=128°-30° C.

後処理

  1. customprepared
  2. customThe center layer was isolated
  3. additiontreated with ligroine (bp=70°-90° C.)
  4. customCrystallization
  5. customthe solid was collected
  6. washwashed with ether
  7. customrecrystallized from acetonitrile

出典と根拠

ORDレコード
ord-48554c8397df4be8a654698e6caa0b45
出典データセット
uspto-grants-1993_03
特許番号
US05196539

関連ノート

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