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Dimethyl Sulfide → Dimethyl 2-pyrrolylsulfonium chloride

HRID 1262952
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HRID 1262952 반응식
[Cl:1][N:2]1[C:6](=O)[CH2:5][CH2:4][C:3]1=O.[CH3:9][S:10][CH3:11].N1C=CC=C1.CCOCC>ClCCl>[Cl-:1].[CH3:9][S+:10]([CH3:11])[C:3]1[NH:2][CH:6]=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 1068Dimethyl SulfideHCID 3283Diethyl EtherHCID 8027PyrroleHCID 31398Chlorosuccinimide

생성물 1

HCID 20456506Dimethyl 2-pyrrolylsulfonium chloride수율 83%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

To a solution of N-chlorosuccinimide (40 g, 0.3 moles) in anhydrous dichloromethane (3 l), cooled to -30° to -40° C. and maintained in a nitrogen atmosphere, was added, with good stirring, α solution of dimethyl sulfide (20.5 g, 0.66 moles) in dichloromethane (125 ml) over a 1 hour period, the temperature being maintained at -30° to -40° C. After a further hour at this temperature, a solution of pyrrole (20 g, 0.3 moles) in dichloromethane (125 ml) was added over a 1 hour period maintaining a temperature of -30° to -40° C. The solution was stirred for a further 2 hours at -30° to -40° C. and then ether (ca 6 l) was added with strong agitation until the precipitation of the product was complete. The solid was collected by filtration, washed three times with ether and dried in vacuo to give a white solid of dimethyl 2-pyrrolylsulfonium chloride (40 g, 83%) which after crystallization from dichloromethane had mp 115°-116° C. dec.

후처리

  1. temperaturemaintained in a nitrogen atmosphere
  2. temperaturethe temperature being maintained at -30° to -40° C
  3. waitAfter a further hour at this temperature
  4. temperaturemaintaining a temperature of -30° to -40° C
  5. filtrationThe solid was collected by filtration
  6. washwashed three times with ether
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-b6c26901718f459c92e9f33f32cf9100
출처 데이터셋
uspto-grants-1984_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04454326

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