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

HRID 248792

反応式

HRID 248792 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°-130° 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-b9170f21b2dc4cc5acce12e4b8c5de13
出典データセット
uspto-grants-1993_05
特許番号
US05212035

関連ノート

読み込み中…