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Morpholine → 2-(1-Naphthylmethylene)-3-(morpholinocarbonyl)propionic acid

HRID 542368
ノート
印刷プレビュー

反応式

HRID 542368 の反応式
[C:1]1([CH:11]=[C:12]2[CH2:17][C:16](=[O:18])[O:15][C:13]2=[O:14])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.[NH:19]1[CH2:24][CH2:23][O:22][CH2:21][CH2:20]1>ClCCl>[C:1]1([CH:11]=[C:12]([CH2:17][C:16]([N:19]2[CH2:24][CH2:23][O:22][CH2:21][CH2:20]2)=[O:18])[C:13]([OH:15])=[O:14])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 8083MorpholineHCID 543164283-[(Naphthalen-1-yl)methylidene]oxolane-2,5-dione

生成物 1

HCID 545343202-(1-Naphthylmethylene)-3-(morpholinocarbonyl)propionic acid収率 80.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 1.00 g of 2-(1-naphthylmethylene)succinic anhydride and 0.37 g of morpholine in 31 ml of dry dichloromethane was stirred for 2 hours at room temperature. The reaction mixture was evaporated under reduced pressure, and the residue was crystallized from a mixture of ethyl acetate, benzene and hexane (1:1:1) to obtain 1.10 g of 2-(1-naphthylmethylene)-3(morpholinocarbonyl)propionic acid as colorless crystals. A solution of 1.00 g of the propionic acid compound was hydrogenated over 0.1 g of a 10% palladium charcoal under a hydrogen atmosphere. After filtration of the catalyst, the filtrate was evaporated under reduced pressure. The residue was crystallized from hexane to give 0.90 g of 2-(1-naphthylmethyl)-3(morpholinocarbonyl)propionic acid as a white powder.

後処理

  1. customThe reaction mixture was evaporated under reduced pressure
  2. customthe residue was crystallized from a mixture of ethyl acetate, benzene and hexane (1:1:1)

出典と根拠

ORDレコード
ord-c60953a3958c4a868244b278f257cc26
出典データセット
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04656269

反応ノート

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