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3-Chloropropionyl chloride → 4-(3-Chloropropionylthiomethyl)-1,3-dithiolane

HRID 1007519
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HRID 1007519 반응식
[SH:1][CH2:2][CH:3]1[CH2:7][S:6][CH2:5][S:4]1.[Cl:8][CH2:9][CH2:10][C:11](Cl)=[O:12]>C1(C)C=CC=CC=1>[Cl:8][CH2:9][CH2:10][C:11]([S:1][CH2:2][CH:3]1[CH2:7][S:6][CH2:5][S:4]1)=[O:12]
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참가 물질

4

반응물 2

HCID 693643-Chloropropionyl chlorideHCID 111827084-Mercaptomethyl-1,3-dithiolane

생성물 1

HCID 114364564-(3-Chloropropionylthiomethyl)-1,3-dithiolane수율 81.7%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Into 500 ml glass reactor equipped with a stirrer and a cooling pipe, 91.2 g (0.60 moles) of 4-mercaptomethyl-1,3-dithiolane (2-1) produced in Example 1 was weighed and poured, and 80.0 g (0.63 moles) of 3-chloropropionic chloride was added dropwise into the reactor at 40° C. over 15 minutes. After reacted at 40° C. for eight hours with stirring, 200 g of toluene was added to the reaction mixture to dissolve the mixture. The mixture then was moved into a separating funnel to be rinsed three times with 300 g of 3 wt. % sodium hydrogen carbonate aqueous solution. Then, after the mixture was rinsed with 300 g of pure water until the water layer became neutral, the organic layer (toluene solution) was taken out. Toluene was evaporated off under reduced pressure, and 119 g of 4-(3-chloropropionylthiomethyl)-1,3-dithiolane was obtained as a transparent and colorless liquid.

후처리

  1. customInto 500 ml glass reactor equipped with a stirrer
  2. additionpoured
  3. customAfter reacted at 40° C. for eight hours
  4. dissolutionto dissolve the mixture
  5. customThe mixture then was moved into a separating funnel
  6. washto be rinsed three times with 300 g of 3 wt. % sodium hydrogen carbonate aqueous solution
  7. washThen, after the mixture was rinsed with 300 g of pure water until the water layer
  8. customToluene was evaporated off under reduced pressure

출처 및 근거

ORD 기록
ord-af0eb7907e1241b6ab21c145029dc57c
출처 데이터셋
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06794471B2

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