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2-Dimethylaminopyrimidine → 1,3-Dioxo-2-(2,6-dioxo-3-fluoropiperidin-3-yl)isoindoline

HRID 618704
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HRID 618704 반응식
[O:1]=[C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[O:11])[N:3]1[C:12]([C:19]([O:21]CC)=O)([F:18])[CH2:13][CH2:14][C:15](O)=[O:16].C(C1NC=CN=1)(C1[NH:27]C=CN=1)=O.CN(C1N=CC=CN=1)C>O1CCCC1>[O:1]=[C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[O:11])[N:3]1[C:12]1([F:18])[CH2:13][CH2:14][C:15](=[O:16])[NH:27][C:19]1=[O:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 5217172-DimethylaminopyrimidineHCID 5250894Bis-(1H-imidazol-2-YL)-methanoneHCID 218479184-(1,3-Dioxoisoindolin-2-yl)-4-(ethoxycarbonyl)-4-fluorobutanoic acid

생성물 1

HCID 98820501,3-Dioxo-2-(2,6-dioxo-3-fluoropiperidin-3-yl)isoindoline

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 4-(1,3-dioxoisoindolin-2-yl)-4-(ethoxycarbonyl)-4-fluorobutanoic acid (0.9 g, 2.8 mmol), carbonyl diimidazole (0.46 g, 2.8 mmol) and dimethylaminopyrimidine (0.68 g, 5.6 mmol) in tetrahydrofuran (30 mL) is heated at reflux for 18 hours. The solvent is removed in vacuo and the residue is stirred with methylene chloride (50 mL) for 10 minutes. The organic layer is washed with water and brine (40 mL each) and dried over sodium sulfate. The solvent is removed in vacuo to give 1,3-dioxo-2-(2,6-dioxo-3-fluoropiperidin-3-yl)isoindoline which is further purified by column chromatography.

후처리

  1. temperatureis heated
  2. temperatureat reflux for 18 hours
  3. customThe solvent is removed in vacuo
  4. washThe organic layer is washed with water and brine (40 mL each)
  5. dry with materialdried over sodium sulfate
  6. customThe solvent is removed in vacuo

출처 및 근거

ORD 기록
ord-19f0cbea206c402299780493cbd1ca8d
출처 데이터셋
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05955476

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