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Sodium Hydroxide → HCID 19348635, 화합물

HRID 1637489
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HRID 1637489 반응식
[OH-].[Na+].[C:3]([C:7]1[CH:12]=[CH:11][C:10]([C:13]([O:15]C)=[O:14])=[CH:9][C:8]=1[NH:17][C:18](=[O:36])[CH2:19][CH:20]([C:26]1[CH:31]=[CH:30][C:29]([O:32][CH3:33])=[CH:28][C:27]=1[O:34][CH3:35])[CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])([CH3:6])([CH3:5])[CH3:4]>CO>[C:3]([C:7]1[CH:12]=[CH:11][C:10]([C:13]([OH:15])=[O:14])=[CH:9][C:8]=1[NH:17][C:18](=[O:36])[CH2:19][CH:20]([C:26]1[CH:31]=[CH:30][C:29]([O:32][CH3:33])=[CH:28][C:27]=1[O:34][CH3:35])[CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])([CH3:4])([CH3:5])[CH3:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

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HCID 14798Sodium HydroxideHCID 19348422N-(2-t-butyl-5-methoxycarbonylphenyl)-3-(2,4-dimethoxyphenyl)octanamide

생성물 1

HCID 19348635HCID 19348635, 화합물수율 71.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

3.5 ml (7.0 mmol) of a 2 N aqueous solution of sodium hydroxide were added to a solution of 1.64 g (3.48 mmol) of N-(2-t-butyl-5-methoxycarbonylphenyl)-3-(2,4-dimethoxyphenyl)octanamide (prepared as described in Preparation 6) in 30 ml of methanol, and the resulting mixture was heated under reflux for 2 hours, after which the solvent was removed by distillation under reduced pressure. The residue was acidified with 2 N aqueous hydrochloric acid and extracted with ethyl acetate. The extract was washed with a saturated aqueous solution of sodium chloride, after which it was dried over anhydrous sodium sulfate. The solvent was removed by distillation under reduced pressure, and the resulting residue was recrystallized from a mixture of ethyl acetate and hexane to give 1.13 g (yield 71%) of the title compound, melting at 153-154° C.

후처리

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 2 hours
  3. customafter which the solvent was removed by distillation under reduced pressure
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with a saturated aqueous solution of sodium chloride
  6. dry with materialafter which it was dried over anhydrous sodium sulfate
  7. customThe solvent was removed by distillation under reduced pressure
  8. customthe resulting residue was recrystallized from a mixture of ethyl acetate and hexane

출처 및 근거

ORD 기록
ord-38789789ba3d47c0a8ba7008dc9c41f3
출처 데이터셋
uspto-grants-2000_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06040339

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