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 15380922、化合物

HRID 610772
ノート
印刷プレビュー

反応式

HRID 610772 の反応式
[H-].[H-].C[CH2-].C[CH2-].[Na+].[Al+3].[CH:9]1([NH2:15])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1.C[O:17][C:18](=O)[CH2:19][CH2:20][CH2:21][CH2:22][N:23]([CH2:35][C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1)[CH2:24][CH2:25][O:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=1[O:33][CH3:34].C(O)(=O)C>C1(C)C=CC=CC=1>[CH:9]1([NH:15][C:18](=[O:17])[CH2:19][CH2:20][CH2:21][CH2:22][N:23]([CH2:35][C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[CH2:24][CH2:25][O:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=2[O:33][CH3:34])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1
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 176Acetic AcidHCID 7965CyclohexylamineHCID 87331Aluminate(1-), diethyldihydro-, sodium (1:1), (T-4)-HCID 15380921HCID 15380921、化合物

生成物 1

HCID 15380922HCID 15380922、化合物収率 47%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒
3 回

反応条件

温度
110 °C

実験手順

A solution of sodium diethyldihydroaluminate (4.44 ml, 8.9 mmole) in a concentration of 2 moles per liter in toluene, is added to a solution of cyclohexylamine (1.76 g, 2.03 ml, 18 mmole) in anhydrous toluene (60 ml). The reaction mixture is heated to 110° C. for 1 hour, then a solution of methyl-5-[benzyl{2-(2-methoxyphenoxy)ethyl}amino]pentanoate (6 g, 16 mmole) in toluene (25 ml) is added dropwise. The mixture is heated under reflux for 3 hours and left for 18 hours at 20° C., then neutralised with a 10% solution of acetic acid. The organic phase is extracted then washed successively with a saturated solution of sodium hydrogen carbonate then with water. After drying over magnesium sulfate and evaporation of the solvents under reduced pressure, the product is purified by flash chromatography over silica gel in a mixture of ethyl acetate/heptane (2/1). 3.3 g (47%) of the desired product are obtained in the form of an oil.

後処理

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 3 hours
  3. extractionThe organic phase is extracted
  4. washthen washed successively with a saturated solution of sodium hydrogen carbonate
  5. dry with materialAfter drying over magnesium sulfate and evaporation of the solvents under reduced pressure
  6. customthe product is purified by flash chromatography over silica gel in a mixture of ethyl acetate/heptane (2/1)

出典と根拠

ORDレコード
ord-770edc398db1457b94fddc89bc2351fa
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05998666

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