Sodium Hydroxide → HCID 178451370, 화합물

HRID 1290999노트

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HRID 1290999 반응식
[C:1]([O:5][C:6]([CH2:8][O:9][C@H:10]1[CH2:15][CH2:14][C@H:13]([N:16]2CN(C)C(=O)N(C)C2)[CH2:12][CH2:11]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[Cl-].[NH4+].[OH-].[Na+]>C(O)(C)(C)C>[NH2:16][C@H:13]1[CH2:14][CH2:15][C@H:10]([O:9][CH2:8][C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:7])[CH2:11][CH2:12]1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 25517Ammonium ChlorideHCID 178481285HCID 178481285, 화합물

생성물 1

HCID 178451370HCID 178451370, 화합물수율 64.5%

시약·촉매·용매 1

HCID 6386tert-Butanol용매

실험 절차

trans-5-[4-[(t-Butoxycabonyl)methyloxy]cyclohexyl]-1,3-dimethylhexahydro-2-oxo-1,3,5-triazine (300mg, 0.879 mmol) was dissolved in t-butanol (5 ml) and a saturated aqueous ammonium chloride solution (5 ml) was added, which was followed by refluxing under heating for 2 hours. The reaction mixture was adjusted to pH 10 with a 1N aqueous sodium hydroxide solution and extracted with benzene. The extract was washed with water and saturated brine, and dried over anhydrous sodium sulfate. After filtration, low boiling matters were distilled away from the filtrate under reduced pressure and the residue was purified by silica gel column chromatography (methylene chloride/methanol=10/1-5/1) to give 130 mg of t-butyl trans-(4-aminocyclohexyloxy)acetate as a colorless solid (57%).

후처리

  1. temperatureby refluxing
  2. temperatureunder heating for 2 hours
  3. extractionextracted with benzene
  4. washThe extract was washed with water and saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationAfter filtration, low boiling matters
  7. distillationwere distilled away from the filtrate under reduced pressure
  8. customthe residue was purified by silica gel column chromatography (methylene chloride/methanol=10/1-5/1)

출처 및 근거

ORD 기록
ord-d64be0aca21f46a78002456b2ac43483
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753670

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