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

Potassium Carbonate → Ethyl 4-[4-(4-trifluoromethylphenoxy)phenoxy]-2-pentenoate

HRID 2286680
ノート
印刷プレビュー

反応式

HRID 2286680 の反応式
[F:1][C:2]([F:18])([F:17])[C:3]1[CH:16]=[CH:15][C:6]([O:7][C:8]2[CH:13]=[CH:12][C:11]([OH:14])=[CH:10][CH:9]=2)=[CH:5][CH:4]=1.Br[CH:20]([CH:27](Br)[CH3:28])[CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[F:1][C:2]([F:17])([F:18])[C:3]1[CH:16]=[CH:15][C:6]([O:7][C:8]2[CH:9]=[CH:10][C:11]([O:14][CH:27]([CH3:28])[CH:20]=[CH:21][C:22]([O:24][CH2:25][CH3:26])=[O:23])=[CH:12][CH:13]=2)=[CH:5][CH:4]=1
参加物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 11430Potassium CarbonateHCID 170230p-(4-(Trifluoromethyl)phenoxy)phenolHCID 12922552Ethyl 3,4-dibromopentanoate

生成物 1

HCID 156921Ethyl 4-[4-(4-trifluoromethylphenoxy)phenoxy]-2-pentenoate収率 82%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

In a reactor, 30 g of ethanol was charged and 12.7 g (0.05 mole) of 4-(4-trifluoromethylphenoxy)phenol, 15.8 g (0.055 mole) of ethyl 3,4-dibromopentanoate, 8.7 g (0.063 mole) of potassium carbonate were charged. They were refluxed for 6 hours to react them. After the reaction, ethanol was distilled off from the reaction mixture and then 50 ml of toluene was added to the resulting mixture, and resulting solution was washed with water and then, the organic phase was washed with 5% hydrochloric acid and with water and then ethyl 3,4-dibromopentanoate and a lower boiling by-products were distilled off at 100° C. under a reduced pressure of 0.02-0.05 mmHg to obtain 15.6 g of ethyl 4-[4-(4-trifluoromethylphenoxy)phenoxy]-2-pentenoate (nD20 1.5175). The yield was 82.0%. The same process was repeated to obtain same compound except using ethyl 3,4-dichloropentanoate 10.9 g (0.055 mole) instead of ethyl 3,4-dibromopentanoate 15.8 g (0.055 mole). The yield was 73.6%.

後処理

  1. temperatureThey were refluxed for 6 hours
  2. customto react them
  3. distillationwas distilled off from the reaction mixture
  4. addition50 ml of toluene was added to the resulting mixture
  5. customresulting solution
  6. washwas washed with water
  7. washthe organic phase was washed with 5% hydrochloric acid and with water
  8. distillationethyl 3,4-dibromopentanoate and a lower boiling by-products were distilled off at 100° C. under a reduced pressure of 0.02-0.05 mmHg

出典と根拠

ORDレコード
ord-1f9d297e08914e4691569c3e88bf165d
出典データセット
uspto-grants-1981_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04267317

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