Diethyl Malonate → 2-(N-tert-butoxycarbonyl-4-butylamino)malonic acid diethyl ester

HRID 1589894ノート

反応式

HRID 1589894 の反応式
[Na].[C:2]([O:10][CH2:11][CH3:12])(=[O:9])[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].[C:13]([O:17][C:18]([NH:20][CH2:21][CH2:22][CH2:23][CH2:24]Cl)=[O:19])([CH3:16])([CH3:15])[CH3:14].CCOC(C)=O.O>C(O)C>[CH2:11]([O:10][C:2](=[O:9])[CH:3]([N:20]([CH2:21][CH2:22][CH2:23][CH3:24])[C:18]([O:17][C:13]([CH3:14])([CH3:15])[CH3:16])=[O:19])[C:4]([O:6][CH2:7][CH3:8])=[O:5])[CH3:12]

参加物

6

反応物 4

HCID 7761Diethyl MalonateHCID 5360545SodiumHCID 19758183tert-Butyl (4-chlorobutyl)carbamateHCID 22728543Water ethylacetate

生成物 1

HCID 867447582-(N-tert-butoxycarbonyl-4-butylamino)malonic acid diethyl ester

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

Metallic sodium (0.28 g, 0.012 mol) is dissolved in absolute ethyl alcohol (EtOH) (9 ml) under nitrogen atmosphere. The mixture is heated to 60° C. and diethyl malonate (3.8 g, 0.024 mol) is then dripped therein. N-tert-butoxycarbonyl-4-chloro-butylamine (2.5 g, 0.012 mol) is then gradually added, at room temperature, to the resulting solution. The reaction mixture is stirred at room temperature for 2 hours and at the reflux temperature for 6 hours, and then poured into a mixture AcOEt/water (100 ml 1/1 v/v). The organic phase which is separated is then washed repeatedly with water and dried over MgSO4.

後処理

  1. customThe organic phase which is separated
  2. washis then washed repeatedly with water
  3. dry with materialdried over MgSO4

出典と根拠

ORDレコード
ord-a51fb4184066454a9b43e42e35018e8f
出典データセット
uspto-grants-1993_04
特許番号
US05200506

反応ノート

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