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

Malonic Acid → Ethyl (Z)-N-(3,4-dichlorobenzyl)-2-ethoxycarbonylindole-3-acrylic acid

HRID 2307930
ノート
印刷プレビュー

反応式

HRID 2307930 の反応式
[C:1](O)(=O)[CH2:2][C:3]([OH:5])=[O:4].C([C:10]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[N:12]([CH2:19][C:20]2[CH:25]=[CH:24][C:23]([Cl:26])=[C:22]([Cl:27])[CH:21]=2)[C:11]=1[C:28]([O:30][CH2:31][CH3:32])=[O:29])=O.N1C=CC=[CH:35][CH:34]=1>N1CCCCC1>[CH2:34]([C:17]1[CH:16]=[CH:15][CH:14]=[C:13]2[C:18]=1[C:10](/[CH:1]=[CH:2]\[C:3]([OH:5])=[O:4])=[C:11]([C:28]([O:30][CH2:31][CH3:32])=[O:29])[N:12]2[CH2:19][C:20]1[CH:25]=[CH:24][C:23]([Cl:26])=[C:22]([Cl:27])[CH:21]=1)[CH3:35]
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 3

HCID 867Malonic AcidHCID 1049PyridineHCID 22603427Ethyl 3-formyl-N-(3,4-dichlorobenzyl)indole-2-carboxylate

生成物 1

HCID 86759582Ethyl (Z)-N-(3,4-dichlorobenzyl)-2-ethoxycarbonylindole-3-acrylic acid収率 19%

試薬・触媒・溶媒 1

HCID 8082Piperidine触媒

反応条件

温度
100 °C

実験手順

Malonic acid (106 mg) and piperidine (1 drop) were added to a solution of ethyl 3-formyl-N-(3,4-dichlorobenzyl)indole-2-carboxylate (315 mg) in pyridine (5 ml) and the reaction stirred at 100° C. overnight. The reaction was concentrated in vacuo and the residue dissolved in ethyl acetate (30 ml), washed with HCl (2M, 30 ml) and water (30 ml), dried (MgSO4) and concentrated in vacuo to give the crude product which was triturated with a mixture of dichloromethane, ethyl acetate and hexane to give the product as a tan coloured solid (68 mg, 19%); NMR d (CD3SOCD3) 1.25 (t, 3H), 4.35 (q, 2H), 5.80 (s, 2H), 6.55 (d, 1H), 6.90 (m, 1H), 7.25-7.45 (m, 3H), 7.50 (m, 1H), 7.60 (m, 1H), 8.05 (m, 1H), 8.35 (d, 1H) 12.24 (s, 1H); M/(−) 416.4 (M−H+).

後処理

  1. concentrationThe reaction was concentrated in vacuo
  2. dissolutionthe residue dissolved in ethyl acetate (30 ml)
  3. washwashed with HCl (2M, 30 ml) and water (30 ml)
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. customto give the crude product which
  7. customwas triturated with a mixture of dichloromethane, ethyl acetate and hexane

出典と根拠

ORDレコード
ord-188324d7df214e5da4edb5b21312741e
出典データセット
uspto-grants-2004_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06833387B1

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