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Pyridine → 2-{[3-(2-Chloroethanesulfonyl)propanoyl]oxy}ethyl prop-2-enoate

HRID 1632529
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HRID 1632529 반응식
[C:1]([O:5][CH2:6][CH2:7][OH:8])(=[O:4])[CH:2]=[CH2:3].[Cl:9][CH2:10][CH2:11][S:12]([CH2:15][CH2:16][C:17](Cl)=[O:18])(=[O:14])=[O:13].N1C=CC=CC=1.C(Cl)(Cl)Cl>O1CCCC1>[C:1]([O:5][CH2:6][CH2:7][O:8][C:17](=[O:18])[CH2:16][CH2:15][S:12]([CH2:11][CH2:10][Cl:9])(=[O:14])=[O:13])(=[O:4])[CH:2]=[CH2:3]
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참가 물질

6

반응물 4

HCID 1049PyridineHCID 6212ChloroformHCID 131652-Hydroxyethyl acrylateHCID 136683973-(2-Chloroethanesulfonyl)propanoyl chloride

생성물 1

HCID 136683982-{[3-(2-Chloroethanesulfonyl)propanoyl]oxy}ethyl prop-2-enoate수율 88.6%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
2회

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온도
5 °C

실험 절차

A mixture of 600 ml of tetrahydrofuran, 45.8 g of hydroxyethyl acrylate, and 72 g of 3-(2-chloroethylsulfonyl)propionic acid chloride was placed in a reactor, and while maintaining the temperature at 5° C. or lower by cooling by ice water, a solution of 31.2 g of pyridine in 100 ml of tetrahydrofuran was added dropwise thereto over a period of 1.75 hours. The resulting mixture was further stirred for 2 hours at room temperature. At the end of the time, the reaction mixture was poured into 2,500 ml of ice water, and extraction was performed four times with 300 ml of chloroform. The organic layer thus extracted was dried over sodium sulfate and concentrated to provide 87 g of 2-[3-(chloroethylsulfonyl)propionyloxy]ethyl acrylate. Yield was 88%.

후처리

  1. customwas placed in a reactor
  2. extractionThe organic layer thus extracted
  3. dry with materialwas dried over sodium sulfate
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-2e3aa30bc6984edc8afd18dcb2d3fc0e
출처 데이터셋
uspto-grants-1984_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04476218

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