ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

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

HRID 1007519
ノート
印刷プレビュー

反応式

HRID 1007519 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 114364564-(3-Chloropropionylthiomethyl)-1,3-dithiolane収率 81.7%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-af0eb7907e1241b6ab21c145029dc57c
出典データセット
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06794471B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート