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 → 2-(beta-Diethylaminoethyl)amino-6-(beta-diethylaminoethyl)aminonitrobenzene dihydrochloride

HRID 981823
ノート
印刷プレビュー

反応式

HRID 981823 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([NH:8][CH2:9][CH2:10][N:11]([CH2:14][CH3:15])[CH2:12][CH3:13])[C:5]([N+:16]([O-:18])=[O:17])=[C:4]([NH:19][CH2:20][CH2:21][N:22]([CH2:25][CH3:26])[CH2:23][CH3:24])[CH:3]=1.C(O)(=O)C.C(O)=O.[ClH:34]>C(N(CC)CC)C.O.C(O)C.[Pd]>[ClH:1].[ClH:34].[CH2:14]([N:11]([CH2:12][CH3:13])[CH2:10][CH2:9][NH:8][C:6]1[CH:7]=[CH:2][CH:3]=[C:4]([NH:19][CH2:20][CH2:21][N:22]([CH2:25][CH3:26])[CH2:23][CH3:24])[C:5]=1[N+:16]([O-:18])=[O:17])[CH3:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 176Acetic AcidHCID 284Formic AcidHCID 313Hydrochloric AcidHCID 200710864-Chloro-2-(beta-diethylaminoethyl)amino-6-(beta-diethylaminoethyl)aminonitrobenzene

生成物 1

HCID 200710842-(beta-Diethylaminoethyl)amino-6-(beta-diethylaminoethyl)aminonitrobenzene dihydrochloride

試薬・触媒・溶媒 4

HCID 23938
Palladium
触媒
HCID 702Ethanol溶媒
HCID 962Water溶媒
HCID 8471Triethylamine溶媒

実験手順

300 mg of palladium at a concentration of 10% on calcium carbonate are added to 0.015 mole (5.8 g) of 4-chloro-2-(β-diethylaminoethyl)amino-6-(β-diethylaminoethyl)aminonitrobenzene in 11.1 ml of triethylamine, after which 2.86 ml of acetic acid and 2.1 ml of formic acid are added dropwise. After the end of the additions, the materials are heated under reflux for 3 hours 30 minutes. The reaction mixture is diluted with 10 ml of water. The catalyst is removed by hot filtration. The filtrate is evaporated to dryness under vacuum. The inorganic salts are precipitated by adding acetone and are removed by filtration. After evaporation of the acetone, an oil is obtained and this, after treatment with a solution of hydrochloric acid in absolute ethanol, leads to the expected product which is isolated by evaporating off the alcohol and precipitating with ethyl ether.

後処理

  1. temperatureAfter the end of the additions, the materials are heated
  2. temperatureunder reflux for 3 hours 30 minutes
  3. customThe catalyst is removed by hot filtration
  4. customThe filtrate is evaporated to dryness under vacuum
  5. customThe inorganic salts are precipitated
  6. additionby adding acetone
  7. customare removed by filtration
  8. customAfter evaporation of the acetone
  9. customan oil is obtained

出典と根拠

ORDレコード
ord-42e6791221cd44598a61d509f76afd30
出典データセット
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04992586

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