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

Acetic Acid → HCID 12766830、化合物

HRID 1577678
ノート
印刷プレビュー

反応式

HRID 1577678 の反応式
[CH2:1]([O:3][C:4]1[CH:11]=[CH:10][C:9]([O:12][CH2:13][CH3:14])=[CH:8][C:5]=1[CH:6]=O)[CH3:2].[C:15]([O:23][CH2:24][CH3:25])(=[O:22])[CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18].N1CCCCC1.C(O)(=O)C>C1C=CC=CC=1.O>[CH2:1]([O:3][C:4]1[CH:11]=[CH:10][C:9]([O:12][CH2:13][CH3:14])=[CH:8][C:5]=1[CH:6]=[C:16]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:15]([O:23][CH2:24][CH3:25])=[O:22])[CH3:2]
参加物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 176Acetic AcidHCID 7761Diethyl MalonateHCID 8082PiperidineHCID 34343142,5-Diethoxybenzaldehyde

生成物 1

HCID 12766830HCID 12766830、化合物収率 92%

試薬・触媒・溶媒 2

HCID 241Benzene溶媒
HCID 962
Water
溶媒
2 回

実験手順

2,5-Diethoxybenzaldehyde (24 g., 0.124 mole) and diethyl malonate (20 g., 0.125 mole) are added to a solution of piperidine (3.0 g.) and glacial acetic acid (6 ml.) in benzene (160 ml.). The mixture is heated under reflux utilizing a Dean-Stark water separater until water ceased to be separated. After 8 hours of distillation 2.3 ml. of water out of a theoretical yield of 2.23 ml. are obtained and the reaction mixture cooled. The cooled reaction mixture is washed with aqueous hydrochloric acid (6 N, 70 ml.) water (70 ml.) and aqueous sodium bicarbonate (5% w/w, 50 ml.). The organic layer is separated, dried over magnesium sulfate, filtered, and the solvent removed under reduced pressure to yield a yellow oil (42.7 g., 0.127 mole, 100%). Trituration with petroleum ether yields diethyl 2,5-Diethoxybenzylidenemalonate (38.4 g., 0.114 mole, 92%) m.p. (from petroleum ether) 52°-53° C. I.R.: 1720 cm- 1 mass spec m/e 336.

後処理

  1. temperatureThe mixture is heated
  2. temperatureunder reflux
  3. customto be separated
  4. distillationAfter 8 hours of distillation 2.3 ml
  5. customare obtained
  6. temperaturethe reaction mixture cooled
  7. customThe cooled reaction mixture
  8. washis washed with aqueous hydrochloric acid (6 N, 70 ml.) water (70 ml.) and aqueous sodium bicarbonate (5% w/w, 50 ml.)
  9. customThe organic layer is separated
  10. dry with materialdried over magnesium sulfate
  11. filtrationfiltered
  12. customthe solvent removed under reduced pressure
  13. customto yield a yellow oil (42.7 g., 0.127 mole, 100%)

出典と根拠

ORDレコード
ord-411643c350b9497c836c5f31ae94a8c0
出典データセット
uspto-grants-1981_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04288608

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