Cesium carbonate → Dimethyl 4-benzyloxy-1-{2-[(tert-butoxycarbonyl)amino]-1-(ethoxycarbonyl)ethyl}-1H-pyrazole-3,5-dicarboxylate

HRID 1453837

반응식

HRID 1453837 반응식
[CH2:1]([O:8][C:9]1[C:10]([C:18]([O:20][CH3:21])=[O:19])=[N:11][NH:12][C:13]=1[C:14]([O:16][CH3:17])=[O:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:22]([O:26][C:27]([NH:29][CH2:30][CH:31](OS(C)(=O)=O)[C:32]([O:34][CH2:35][CH3:36])=[O:33])=[O:28])([CH3:25])([CH3:24])[CH3:23].C([O-])([O-])=O.[Cs+].[Cs+]>CC#N>[CH2:1]([O:8][C:9]1[C:13]([C:14]([O:16][CH3:17])=[O:15])=[N:12][N:11]([CH:31]([C:32]([O:34][CH2:35][CH3:36])=[O:33])[CH2:30][NH:29][C:27]([O:26][C:22]([CH3:25])([CH3:23])[CH3:24])=[O:28])[C:10]=1[C:18]([O:20][CH3:21])=[O:19])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 57528491dimethyl 4-benzyloxy-1H-pyrazole-3,5-dicarboxylateHCID 86617817Ethyl 3-[(tert-butoxycarbonyl)amino]-2-(methylsulfonyloxy)propanoate

생성물 1

HCID 68952340Dimethyl 4-benzyloxy-1-{2-[(tert-butoxycarbonyl)amino]-1-(ethoxycarbonyl)ethyl}-1H-pyrazole-3,5-dicarboxylate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
50 °C

실험 절차

To a solution of dimethyl 4-benzyloxy-1H-pyrazole-3,5-dicarboxylate (4.0 g, 13.8 mmol) and ethyl 3-[(tert-butoxycarbonyl)amino]-2-(methylsulfonyloxy)propanoate (4.29 g, 13.8 mmol) in anhydrous CH3CN (200 mL) was added Cs2CO3 (4.49 g, 13.8 mmol). The mixture was heated to 50° C. overnight, cooled to room temperature, and filtered. The filtrate was concentrated in vacuo to afford the title product as a pale yellow oil. ES MS (M+H)=506.

후처리

  1. temperaturecooled to room temperature
  2. filtrationfiltered
  3. concentrationThe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-3551b1420a9d47008d3cdb63cd312737
출처 데이터셋
uspto-grants-2009_01
특허 번호
US07476666B2

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