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Ethyl chloroformate → 5-(1,1-Dimethylethyl) 1-ethyl hexahydropyrrolo[3,4-b]pyrrole-1,5-dicarboxylate

HRID 1975002
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반응식

HRID 1975002 반응식
[CH:1]12[CH2:8][N:7]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:6][CH:5]1[CH2:4][CH2:3][NH:2]2.[OH-].[Na+].Cl[C:19]([O:21][CH2:22][CH3:23])=[O:20]>C1(C)C=CC=CC=1.O>[CH:1]12[CH2:8][N:7]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:6][CH:5]1[CH2:4][CH2:3][N:2]2[C:19]([O:21][CH2:22][CH3:23])=[O:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 10928Ethyl chloroformateHCID 14798Sodium HydroxideHCID 225622051,1-Dimethylethyl hexahydropyrrolo[3,4-b]pyrrole-5(1H)-carboxylate

생성물 1

HCID 191009335-(1,1-Dimethylethyl) 1-ethyl hexahydropyrrolo[3,4-b]pyrrole-1,5-dicarboxylate

시약·촉매·용매 2

HCID 962Water용매HCID 1140
Toluene
용매

실험 절차

13 g (61.2 mmol) of tert.-butyl 2,7-diazabicyclo[3.3.0]octane-7-carboxylate are dissolved in 100 ml of toluene, a solution of 3 g of sodium hydroxide in 20 ml of water is added, and 7 g (64.5 mmol) of ethyl chloroformate are added dropwise at room temperature. The mixture is stirred for 3 hours at room temperature, and the aqueous phase is separated off and extracted twice using 100 ml portions of methylene chloride. The organic solutions are dried over magnesium sulphate, concentrated and distilled.

후처리

  1. customthe aqueous phase is separated off
  2. extractionextracted twice
  3. dry with materialThe organic solutions are dried over magnesium sulphate
  4. concentrationconcentrated
  5. distillationdistilled

출처 및 근거

ORD 기록
ord-8509c70b9430404b8dd95226c359c9f5
출처 데이터셋
uspto-grants-1994_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05284855

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