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Hydrogen chloride-ethyl acetate → HCID 66976532, 화합물

HRID 1022609
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HRID 1022609 반응식
[C:1]([NH:4][CH2:5][C@H:6]1[C@H:12]([C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[C:15]([Cl:20])[CH:14]=2)[O:11][CH2:10][CH2:9][N:8](C(OC(C)(C)C)=O)[CH2:7]1)(=[O:3])[CH3:2].C(OCC)(=O)C.Cl>C(O)C>[Cl:20][C:15]1[CH:14]=[C:13]([C@@H:12]2[O:11][CH2:10][CH2:9][NH:8][CH2:7][C@H:6]2[CH2:5][NH:4][C:1](=[O:3])[CH3:2])[CH:18]=[CH:17][C:16]=1[Cl:19]
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참가 물질

4

반응물 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 66976309HCID 66976309, 화합물

생성물 1

HCID 66976532HCID 66976532, 화합물수율 60.4%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of tert-butyl (6R,7R)-6-[(acetylamino)methyl]-7-(3,4-dichlorophenyl)-1,4-oxazepane-4-carboxylate (160 mg) in ethanol (0.5 mL) was added 4.0 M hydrogen chloride-ethyl acetate solution (3 mL), and the mixture was stirred at room temperature for 1.5 hr. The solvent was evaporated under reduced pressure. To the residue was added 1 N aqueous sodium hydroxide solution, and the mixture was extracted twice with ethyl acetate. The combined organic layers were washed with brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was dissolved in ethanol, and a solution of fumaric acid (39.3 mg) in ethanol was added. The solvent was evaporated under reduced pressure. The obtained crystals were recrystallized from ethanol-ethyl acetate to give the title compound (73.5 mg) as colorless crystals.

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. additionTo the residue was added 1 N aqueous sodium hydroxide solution
  3. extractionthe mixture was extracted twice with ethyl acetate
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. dissolutionThe residue was dissolved in ethanol
  8. additiona solution of fumaric acid (39.3 mg) in ethanol was added
  9. customThe solvent was evaporated under reduced pressure
  10. customThe obtained crystals were recrystallized from ethanol-ethyl acetate

출처 및 근거

ORD 기록
ord-23f8f66375d74b9f88b70b8bd177ae1a
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08722662B2

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