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

HRID 248792

반응식

HRID 248792 반응식
[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

참가 물질

5

반응물 3

HCID 962Water2회HCID 31389Sodium 3-nitrobenzenesulfonateHCID 19762119N-(2-benzoyloxyethyl)pyridinium bromide

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b9170f21b2dc4cc5acce12e4b8c5de13
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05212035

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