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

HRID 1396840노트

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HRID 1396840 반응식
[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]

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 2205541,2-Bis(phenylmethyl) 1,2-hydrazinedicarboxylateHCID 5107723tert-Butyl 2,4-dibromobutyrate

생성물 1

HCID 683499043-(1,1-Dimethylethyl) 1,2-bis(phenylmethyl) 1,2,3-pyrazolidinetricarboxylate수율 102.8%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
50 °C

실험 절차

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.

후처리

  1. customwere completely consumed
  2. temperatureThe mixture solution was cooled to room temperature
  3. filtrationA filtration
  4. customto remove some undissolved materials
  5. concentrationThe filtrate was concentrated under vacuum

출처 및 근거

ORD 기록
ord-df41402dcf2c49969e18cb4fb1077656
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08901119B2

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