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

HRID 1589894노트

반응식

HRID 1589894 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
60 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-a51fb4184066454a9b43e42e35018e8f
출처 데이터셋
uspto-grants-1993_04
특허 번호
US05200506

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