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

Benzenepropanoic acid → N-(3-phenylpropionyl)-L-proline benzyl ester

HRID 1720506
ノート
印刷プレビュー

反応式

HRID 1720506 の反応式
Cl.[CH2:2]([O:9][C:10](=[O:16])[C@@H:11]1[CH2:15][CH2:14][CH2:13][NH:12]1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C(N(CC)CC)C.[C:24]1([CH2:30][CH2:31][C:32](O)=[O:33])[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.C1CCC(N=C=NC2CCCCC2)CC1>C(Cl)Cl>[CH2:2]([O:9][C:10](=[O:16])[C@@H:11]1[CH2:15][CH2:14][CH2:13][N:12]1[C:32](=[O:33])[CH2:31][CH2:30][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1
参加物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 107Benzenepropanoic acidHCID 8471TriethylamineHCID 10868DicyclohexylcarbodiimideHCID 2733413Proline benzyl ester hydrochloride

生成物 1

HCID 45139423N-(3-phenylpropionyl)-L-proline benzyl ester収率 93.5%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

To a solution of L-proline benzyl ester hydrochloride (20.0 g) in methylene chloride (250 ml) were added triethylamine (11.5 ml), 3-phenylpropionic acid (13.7 g) and DCC (18.8 g) under ice-cooling, and the mixture was stirred for 2 hours. After stirring at room temperature for 14 hours, the insoluble material was filtered off, and the filtrate was concentrated. The residue was dissolved in ethyl acetate, and the solution was washed with 1N hydrochloric acid, saturated aqueous solution of sodium bicarbonate and saturated brine, dried over anhydrous magnesium sulfate, and concentrated. The residue was purified by silica gel column chromatography (eluate: hexane-ethyl acetate). To thus-obtained N-(3-phenylpropionyl)-L-proline benzyl ester (26.1 g) in 1% water-containing methanol (200 ml) was added 10% Pd--C (3.0 g), and the mixture was stirred at room temperature under hydrogen atmosphere for 2.5 hours. The catalyst was filtered off, and the filtrate was concentrated to give 17.4 g of the title compound.

後処理

  1. temperaturecooling
  2. stirringAfter stirring at room temperature for 14 hours
  3. filtrationthe insoluble material was filtered off
  4. concentrationthe filtrate was concentrated
  5. dissolutionThe residue was dissolved in ethyl acetate
  6. washthe solution was washed with 1N hydrochloric acid, saturated aqueous solution of sodium bicarbonate and saturated brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated
  9. customThe residue was purified by silica gel column chromatography (eluate: hexane-ethyl acetate)

出典と根拠

ORDレコード
ord-9036e7c8033c48ff811aedeed9fb48eb
出典データセット
uspto-grants-1996_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05506256

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