1,2-Dichlorobenzene → p-Toluenesulfonic acid

HRID 66771

반응식

HRID 66771 반응식
CSC1C=CC(C)=CC=1OCC1NCCN=1.CSC1C=CC(C)=CC=1OCC#N.[C:30]1([CH3:40])[CH:35]=[CH:34][C:33]([S:36]([OH:39])(=[O:38])=[O:37])=[CH:32][CH:31]=1.C(N)CN.ClC1C=CC=CC=1Cl>C(Cl)Cl>[CH3:40][C:30]1[CH:35]=[CH:34][C:33]([S:36]([OH:39])(=[O:38])=[O:37])=[CH:32][CH:31]=1

참가 물질

6

반응물 4

HCID 72391,2-DichlorobenzeneHCID 2250301,2-Ethanediamine, 4-methylbenzenesulfonate (1:?)HCID 705471844-Methylthio-m-tolyloxyacetonitrileHCID 705477522-((4-(Methylthio)-m-tolyloxy)methyl)-2-imidazoline

생성물 1

HCID 6101p-Toluenesulfonic acid수율 188.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

The product, 2-((4-(methylthio)-m-tolyloxy)methyl)-2-imidazoline, was prepared by heating 19.3 g of 4-methylthio-m-tolyloxyacetonitrile, 23.3 g of ethylenediamine p-toluenesulfonate and 75 ml of 1,2-dichlorobenzene substantially as described in previous examples. Upon cooling the reaction mixture, diluting with CH2Cl2 and filtering, 32.5 g of p-toluenesulfonate salt was obtained. The p-toluenesulfonate salt was then slurried in water and CH2Cl2 and then basified. The CH2Cl2 layer was separated and the aqueous layer extracted with chloroform. The extracts were combined, treated with diatomaceous earth and activated charcoal and then filtered. The filtrate was taken to dryness, which gave 13.5 g of the product, 2-((4-(methylthio)-m-tolyloxy)methyl)-2-imidazoline as a white solid, m.p. 102°-104° C.

후처리

  1. temperatureUpon cooling the reaction mixture
  2. filtrationfiltering

출처 및 근거

ORD 기록
ord-9f359e437e9c4394970d53471b23e6ed
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04343808

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