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Cesium carbonate → HCID 59279885, 화합물

HRID 2045707
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HRID 2045707 반응식
C([O-])([O-])=O.[Cs+].[Cs+].BrC1C=CC(S([O:17][C@@H:18]2[CH2:22][N:21]([C:23]([O:25][C:26]([CH3:29])([CH3:28])[CH3:27])=[O:24])[C@H:20]([C:30]([O:32][CH3:33])=[O:31])[CH2:19]2)(=O)=O)=CC=1.[Br:34][C:35]1[CH:36]=[C:37]2[C:42](=[CH:43][C:44]=1[O:45][CH3:46])[NH:41][C:40](=[O:47])[CH:39]=[C:38]2O>CN1C(=O)CCC1>[Br:34][C:35]1[CH:36]=[C:37]2[C:42](=[CH:43][C:44]=1[O:45][CH3:46])[NH:41][C:40](=[O:47])[CH:39]=[C:38]2[O:17][C@H:18]1[CH2:22][N:21]([C:23]([O:25][C:26]([CH3:27])([CH3:28])[CH3:29])=[O:24])[C@H:20]([C:30]([O:32][CH3:33])=[O:31])[CH2:19]1
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참가 물질

5

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HCID 10796Cesium carbonateHCID 565904841-(tert-Butyl) 2-methyl (2S,4S)-4-(((4-bromophenyl)sulfonyl)oxy)pyrrolidine-1,2-dicarboxylateHCID 592798516-Bromo-4-hydroxy-7-methoxyquinolin-2(1H)-one

생성물 1

HCID 59279885HCID 59279885, 화합물수율 53%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone
용매

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온도
60 °C

실험 절차

Cs2CO3 (8.42 g, 25.8 mmol) was added to a solution of 1-tert-butyl 2-methyl (2S,4S)-4-{[(4-bromophenyl)sulfonyl]oxy}pyrrolidine-1,2-dicarboxylate (4 g, 8.61 mmol) and the product from step 1 (3.49 g, 12.92 mmol) in NMP (86 ml) under nitrogen. The mixture was then heated to 60° C. After 6.5 h, the reaction was extracted with water and EtOAc. The organic layer was extracted with water and brine and dried over MgSO4. The solvent was then removed in vacuo. The crude product (6.5 g) was purified on silica (gradient elution, 0-100% EtOAc/hexanes, and then 0-5% MeOH/DCM) to yield 2.26 g (53%) of the title compound. LRMS ESI+ ((M-Boc)+H)+ 397.3/399.3.

후처리

  1. extractionthe reaction was extracted with water and EtOAc
  2. extractionThe organic layer was extracted with water and brine
  3. dry with materialdried over MgSO4
  4. customThe solvent was then removed in vacuo
  5. customThe crude product (6.5 g) was purified on silica (
  6. washgradient elution, 0-100% EtOAc/hexanes

출처 및 근거

ORD 기록
ord-bef46001d7c84355aa519de1f1fe297d
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08591878B2

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