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Hydrochloric Acid → HCID 68643997, 화합물

HRID 2388703
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HRID 2388703 반응식
Cl.C([N:5]1[CH2:10][CH2:9][C:8]2(N3CCCC3)[O:11][N:12]=[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:7]2[CH:6]1[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)(=O)C>>[C:24]1([CH:6]2[C:7]3[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[N:12][O:11][C:8]=3[CH2:9][CH2:10][NH:5]2)[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 313Hydrochloric AcidHCID 68643979HCID 68643979, 화합물

생성물 1

HCID 68643997HCID 68643997, 화합물수율 50%

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온도
130 °C

실험 절차

Conc. HCl (12 ml) was added to ethyl 5-acetyl-4-phenyl-7a-(pyrrolidin-1-yl)-3a,4,5,6,7,7a-hexahydroisoxazolo[4,5-c]pyridine-3-carboxylate (2 g) at 0° C., and the reaction mixture was heated to 130° C. for 5 h. The hydrochloric acid was evaporated under reduced pressure and the residue was dissolved in dichloromethane and basified with sodium carbonate solution. The organic layer was separated and the aqueous layer was extracted with dichloromethane. The combined organic layers were washed with brine solution and dried over sodium sulfate. The solvent was evaporated under reduced pressure to give the crude compound which was used in the next step without further purification. Yield: 50%.

후처리

  1. customThe hydrochloric acid was evaporated under reduced pressure
  2. dissolutionthe residue was dissolved in dichloromethane
  3. customThe organic layer was separated
  4. extractionthe aqueous layer was extracted with dichloromethane
  5. washThe combined organic layers were washed with brine solution
  6. dry with materialdried over sodium sulfate
  7. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-3bfc85d0a6ef4d5da6a9f878f7aee0a4
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08268814B2

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