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

Ethyl Acetoacetate → 3-(2'-Oxo-3'-ethoxycarbonylbutyl)-benzophenone

HRID 1731182
ノート
印刷プレビュー

反応式

HRID 1731182 の反応式
[CH3:1][CH2:2][O-:3].[Na+].[Na].[C:6]([CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])(=O)C.BrC[C:17]1[CH:18]=[C:19]([CH:28]=[CH:29][CH:30]=1)[C:20]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)=[O:21]>C1C=CC=CC=1>[O:3]=[C:2]([CH:9]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH3:6])[CH2:1][C:24]1[CH:23]=[C:22]([CH:27]=[CH:26][CH:25]=1)[C:20]([C:19]1[CH:18]=[CH:17][CH:30]=[CH:29][CH:28]=1)=[O:21]
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

6

反応物 4

HCID 8868Ethyl AcetoacetateHCID 895863-(Bromomethyl)benzophenoneHCID 2723922Sodium ethoxideHCID 5360545Sodium

生成物 1

HCID 214956583-(2'-Oxo-3'-ethoxycarbonylbutyl)-benzophenone

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

反応条件

温度
100 °C

実験手順

Dry sodium ethylate prepared from 2.51 g of sodium was added to 125 ml of anhydrous benzene and 13.5 ml of ethyl acetylacetate at 20° C and after heating at 100° C for 15 minutes, 27.5 g of 3-bromomethyl-benzophenone were added all at once. The reaction mixture was refluxed for 3 hours and after cooling to 20° C, the benzene solution was washed twice with 25 ml of 2N hydrochloric acid and then with water until the wash water was neutral. The solution was dried over sodium sulfate and evaporated to dryness under reduced pressure to obtain 33.8 g of raw product which was chromatographed over silica gel and was eluted with a 50-50 mixture of ether-petroleum ether (B.P. of 40°-60° C) to obtain 15.3 g of 3-(2'-oxo-3'-ethoxycarbonyl-butyl)-benzophenone in the form of a marron resin which was used as is for the next step.

後処理

  1. temperatureThe reaction mixture was refluxed for 3 hours
  2. temperatureafter cooling to 20° C
  3. washthe benzene solution was washed twice with 25 ml of 2N hydrochloric acid
  4. dry with materialThe solution was dried over sodium sulfate
  5. customevaporated to dryness under reduced pressure
  6. customto obtain 33.8 g of raw product which
  7. customwas chromatographed over silica gel
  8. washwas eluted with a 50-50 mixture of ether-petroleum ether (B.P. of 40°-60° C)

出典と根拠

ORDレコード
ord-d549663478cf437db3d6959472429d59
出典データセット
uspto-grants-1976_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03995056

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