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

Oxalyl chloride → Ethyl 5-(trifluoromethyl)-1-benzothiophene-2-carboxylate

HRID 2271308
ノート
印刷プレビュー

反応式

HRID 2271308 の反応式
[C:1](Cl)(=[O:5])[C:2](Cl)=O.[F:7][C:8]([F:22])([F:21])[C:9]1[CH:20]=[CH:19][C:12]2[S:13][C:14]([C:16](O)=[O:17])=[CH:15][C:11]=2[CH:10]=1>C(O)C>[F:21][C:8]([F:7])([F:22])[C:9]1[CH:20]=[CH:19][C:12]2[S:13][C:14]([C:16]([O:5][CH2:1][CH3:2])=[O:17])=[CH:15][C:11]=2[CH:10]=1
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 65578Oxalyl chlorideHCID 27830435-(Trifluoromethyl)-1-benzothiophene-2-carboxylic acid

生成物 1

HCID 70982228Ethyl 5-(trifluoromethyl)-1-benzothiophene-2-carboxylate収率 74.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Then, 254 mg of oxalyl chloride was added to a mixture of 400 mg of 5-(trifluoromethyl)benzo[b]thiophene-2-carboxylic acid and 20 ml of ethanol while ice-cooling, and the mixture was stirred for 6 hours under reflux. The reaction mixture was cooled to room temperature, and then concentrated under reduced pressure. To the residue was added chloroform, and then the organic layer was washed with saturated aqueous sodium bicarbonate solution and saturated aqueous sodium chloride solution, dried over magnesium sulfate, and then concentrated under reduced pressure to obtain 330 mg of ethyl 5-(trifluoromethyl)benzo[b]thiophene-2-carboxylate (the present compound 5).

後処理

  1. temperaturecooling
  2. temperatureunder reflux
  3. concentrationconcentrated under reduced pressure
  4. additionTo the residue was added chloroform
  5. washthe organic layer was washed with saturated aqueous sodium bicarbonate solution and saturated aqueous sodium chloride solution
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-acfe27147c714dbf9aa70e020235efe9
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09119396B2

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