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Triclosan → 5-Chloro-2-(2,4-dichlorophenoxy)phenyl prop-2-enoate

HRID 991379
ノート
印刷プレビュー

反応式

HRID 991379 の反応式
[CH:1]1[C:6]([Cl:7])=[CH:5][C:4]([OH:8])=[C:3]([O:9][C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][C:11]=2[Cl:17])[CH:2]=1.C(N(CC)CC)C.[C:25](Cl)(=[O:28])[CH:26]=[CH2:27]>O1CCCC1>[CH2:27]=[CH:26][C:25]([O:8][C:4]1[CH:5]=[C:6]([Cl:7])[CH:1]=[CH:2][C:3]=1[O:9][C:10]1[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][C:11]=1[Cl:17])=[O:28]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 5564TriclosanHCID 8471TriethylamineHCID 13140Acryloyl chloride2 回

生成物 1

HCID 673466385-Chloro-2-(2,4-dichlorophenoxy)phenyl prop-2-enoate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
20 °C

実験手順

Irgasan® DP300 5-chloro-2-(2,4-dichlorophenol)(triclosan), 23.5 g (0.081 mol) was dissolved in 300 ml of dry tetrahydrofuran in a 1-l jacketed kettle with agitator, addition funnel and reflux condenser. Then 10.6 ml of triethylamine was added to the solution with agitation. To the resulting solution was added dropwise 6.68 (0.0738 mol) g of acryloyl chloride. The reaction temperature was maintained at 20° C. with a circulating cooling bath. After the addition of acryloyl chloride was completed, the agitation and temperature conditions were maintained for 5 hours. Then the reaction product was kept overnight at room temperature, filtered to remove solid triethylamine hydrochloride and the filtrate rotovapped at room temperature under 100-110 mm Hg to concentrate the product. The remaining solution was dissolved in 100 ml heptane and washed with 5% Na2CO3 solution in Dl water until basic; then with Dl water until neutral. The heptane solution of the product was dried with MgSO4 in a refrigerator overnight, and filtered. The filtrate contained 25.3% triclosan acrylate as determined by bromination. FTIR spectrum confirmed the presence of the unsaturated ester of a phenol (1753 cm−1).

後処理

  1. temperaturereflux condenser
  2. temperaturea circulating cooling bath
  3. temperaturethe agitation and temperature conditions were maintained for 5 hours
  4. filtrationfiltered
  5. customto remove solid triethylamine hydrochloride
  6. customrotovapped at room temperature under 100-110 mm Hg
  7. concentrationto concentrate the product
  8. dissolutionThe remaining solution was dissolved in 100 ml heptane
  9. washwashed with 5% Na2CO3 solution in Dl water until basic
  10. dry with materialThe heptane solution of the product was dried with MgSO4 in a refrigerator overnight
  11. filtrationfiltered

出典と根拠

ORDレコード
ord-541733ca58234a7d962701877abd65d5
出典データセット
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06464961B2

反応ノート

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