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Acetic Acid → HCID 58313094, 화합물

HRID 1800779
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HRID 1800779 반응식
CC([Si](C)(C)[O:6][CH:7]1[CH2:31][CH2:30][C:10]2([CH2:14][N:13]([C:15]([O:17][CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[O:16])[CH:12]([C:25]([O:27][CH2:28][CH3:29])=[O:26])[CH2:11]2)[CH2:9][CH2:8]1)(C)C.C(O)(=O)C.CCCC[N+](CCCC)(CCCC)CCCC.[F-].C1C=CN=CC=1.F.C([O-])(O)=O.[Na+].C(=O)([O-])[O-].[K+].[K+]>C1COCC1>[OH:6][CH:7]1[CH2:8][CH2:9][C:10]2([CH2:14][N:13]([C:15]([O:17][CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[O:16])[CH:12]([C:25]([O:27][CH2:28][CH3:29])=[O:26])[CH2:11]2)[CH2:30][CH2:31]1
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HCID 176Acetic AcidHCID 11430Potassium CarbonateHCID 64774Pyridine, hydrofluoride (1:1)HCID 516892Sodium BicarbonateHCID 2724141Tetrabutylammonium FluorideHCID 583131673-Ethyl 2-(phenylmethyl) 8-{[(1,1-dimethylethyl)(dimethyl)silyl]oxy}-2-azaspiro[4.5]decane-2,3-dicarboxylate

생성물 1

HCID 58313094HCID 58313094, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of 3-ethyl 2-(phenylmethyl) 8-{[(1,1-dimethylethyl)(dimethyl)silyl]oxy}-2-azaspiro[4.5]decane-2,3-dicarboxylate (111) (5.73 g, 12.05 mmol) in THF (60 mL) was added glacial acetic acid (1.38 mL, 24.0 mmol) followed by TBAF (24 mL) as a 1 M solution in THF. The reaction was stirred at room temperature for 72 h. The reaction was partitioned between EtOAc and water (250 mL) each, the organic layer was separated and washed with saturated NaHCO3 (100 mL) and dried (MgSO4) and concentrated in vacuo. The reaction was found to be incomplete by TLC. The residue was dissolved in dry THF (60 mL), cooled to 0° C. and treated with HF-pyridine (1.6 mL, 18.0 mmol), warmed to room temperature and stirred for 2 h under nitrogen. The reaction was poured into saturated NaHCO3 (100 mL) and solid potassium carbonate was added until gas evolution ceased. Extracted with EtOAc (2×150 mL), the organic layers were combined and washed with 0.1 N HCl (100 mL), dried (MgSO4) and concentrated in vacuo to afford the title compound in quantitative yield as a yellow oil which was used in subsequent reactions without additional purification.

후처리

  1. customThe reaction was partitioned between EtOAc and water (250 mL) each, the organic layer
  2. customwas separated
  3. washwashed with saturated NaHCO3 (100 mL)
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. dissolutionThe residue was dissolved in dry THF (60 mL)
  7. temperaturecooled to 0° C.
  8. temperaturewarmed to room temperature
  9. stirringstirred for 2 h under nitrogen
  10. additionwas added until gas evolution
  11. extractionExtracted with EtOAc (2×150 mL)
  12. washwashed with 0.1 N HCl (100 mL)
  13. dry with materialdried (MgSO4)
  14. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-0bec3b8d56db455c96e63891dd546639
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08344155B2

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