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

Hydrochloric Acid → 1-(3,4-Dimethoxyphenyl)-4,4,4-trifluorobutane-1,3-dione

HRID 2210635
ノート
印刷プレビュー

反応式

HRID 2210635 の反応式
C[O-].[Na+].[F:4][C:5]([F:12])([F:11])[C:6]([O:8]CC)=O.[CH3:13][C:14]([C:16]1[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[C:18]([O:24][CH3:25])[CH:17]=1)=[O:15].Cl>C1(C)C=CC=CC=1.O>[CH3:25][O:24][C:18]1[CH:17]=[C:16]([C:14](=[O:15])[CH2:13][C:6](=[O:8])[C:5]([F:4])([F:11])[F:12])[CH:21]=[CH:20][C:19]=1[O:22][CH3:23]
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

7

反応物 4

HCID 313Hydrochloric AcidHCID 9794Ethyl trifluoroacetateHCID 143283,4-Dimethoxyphenyl methyl ketoneHCID 10942334Sodium Methoxide

生成物 1

HCID 69172031-(3,4-Dimethoxyphenyl)-4,4,4-trifluorobutane-1,3-dione収率 96%

試薬・触媒・溶媒 2

HCID 962Water
溶媒
HCID 1140Toluene溶媒2 回

反応条件

温度
50 °C

実験手順

216 g (4 mol) of anhydrous sodium methylate and 3.5 l of toluene are introduced into a 10 liter round-bottomed flask and, under vigorous stirring, 705 g (5 mol) of ethyl trifluoroacetate are then run in; the temperature rises slowly to 30° C. After cooling in an ice bath, a solution of 720 g (4 mol) of 3,4-dimethoxyacetophenone in 0.5 l of toluene is added dropwise to the reaction mixture; a white precipitate slowly forms. The mixture is next left stirred overnight and then heated to 50° C. for three hours. After cooling, 2 1 of water and 330 ml of concentrated hydrochloric acid are added, the organic phase is separated off after settling has taken place, dried over magnesium sulphate, filtered and evaporated to obtain 1060 g (96%) of a yellow solid melting at 87°-89° C.

後処理

  1. customrises slowly to 30° C
  2. temperatureAfter cooling in an ice bath
  3. waitThe mixture is next left
  4. temperatureAfter cooling
  5. customthe organic phase is separated off after settling
  6. dry with materialdried over magnesium sulphate
  7. filtrationfiltered
  8. customevaporated

出典と根拠

ORDレコード
ord-ced4b3146bce44aeb88c5de9966e7e24
出典データセット
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05459262

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート