Cesium carbonate → 3-(1,1-Dimethylethyl) 1,2-bis(phenylmethyl) 1,2,3-pyrazolidinetricarboxylate

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Reaktionsgleichung

[CH2:1]([O:8][C:9]([NH:11][NH:12][C:13]([O:15][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)=[O:14])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[Cs+].[Cs+].Br[CH:30]([CH2:38][CH2:39]Br)[C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32]>C(#N)C>[N:11]1([C:9]([O:8][CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)=[O:10])[CH2:39][CH2:38][CH:30]([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[N:12]1[C:13]([O:15][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)=[O:14]

Komponenten

Reaktionsbedingungen

Temperatur: 50 °C

Versuchsvorschrift

A solution of bis(benzyloxycarbonyl)hydrazine (2.65 g, 8.83 mol) in acetonitrile (30 L) was charged into 100 L-reactor. Cesium carbonate (6.00 kg, 18.4 mol) and tert-butyl 2,4-dibromobutyrate (2.65 kg, 8.83 mol) were added into the above solution. The mixture solution was heated at 50° C. for 2.5 h until the two starting materials were completely consumed. The mixture solution was cooled to room temperature. A filtration was performed to remove some undissolved materials. The filtrate was concentrated under vacuum to afford product (4000 g crude product) as a brown oil.

Aufarbeitung

customwere completely consumed
temperatureThe mixture solution was cooled to room temperature
filtrationA filtration
customto remove some undissolved materials
concentrationThe filtrate was concentrated under vacuum

Quellen und Nachweise

ORD-Eintrag: ord-df41402dcf2c49969e18cb4fb1077656
Quelldatensatz: uspto-grants-2014_12
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08901119B2

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