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

Methyl Acrylate → HCID 21079442、化合物

HRID 1375105
ノート
印刷プレビュー

反応式

HRID 1375105 の反応式
[CH3:1][CH:2]([CH3:11])[C:3](=[O:10])[CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].[C:12]([O:16][CH3:17])(=[O:15])[CH:13]=[CH2:14]>C1CCN2C(=NCCC2)CC1.C1CCCCC1>[CH3:17][O:16][C:12](=[O:15])[CH2:13][CH2:14][C:4]([C:5]([O:7][CH2:8][CH3:9])=[O:6])([C:3](=[O:10])[CH:2]([CH3:1])[CH3:11])[CH2:3][CH2:4][C:5]([O:7][CH3:8])=[O:6]
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 2

HCID 7294Methyl AcrylateHCID 81583Ethyl isobutyrylacetate

生成物 1

HCID 21079442HCID 21079442、化合物収率 112.5%

試薬・触媒・溶媒 2

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-ene触媒HCID 8078Cyclohexane溶媒

反応条件

温度
60 °C

実験手順

12.0 g (0.08 mol) of ethyl 4-methyl-3-oxo-pentanoate and 0.5 g (0.003 mol) of DBU were placed in a three necked round bottom flask, equipped-with dropping funnel and reflux condenser. At room temperature, 16.0 g (0.18 mol) of methyl acrylate was slowly added drop by drop. After the exothermal behavior of the reaction leveled off, the reaction mixture was stirred at 60° C. for an additional two hours. The mixture was poured into cyclohexane and was washed with diluted hydrochloric acid and was subsequently washed with distilled water until the aqueous layer was neutral. The organic layer was dried over sodium sulfate, the solvent was removed, and the addition product was isolated by fractional distillation in a vacuum. 15.0 g (0.045 mol) of 4-(ethoxycarbonyl)-4-(2-methyl-1-oxopropyl)-heptanedioic acid 1,7-dimethyl ester was obtained (yield: 56%; boiling point: 145° C. at 0.02 mbar; colorless).

後処理

  1. temperaturereflux condenser
  2. customAt room temperature
  3. washwas washed with diluted hydrochloric acid
  4. washwas subsequently washed with distilled water until the aqueous layer
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. customthe solvent was removed
  7. customthe addition product was isolated by fractional distillation in a vacuum

出典と根拠

ORDレコード
ord-48f4518df1404a2dae24378b0559ee6a
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07166648B2

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