Ethyl bromoacetate → HCID 19689412, 화합물

HRID 583102노트

반응식

HRID 583102 반응식
[CH2:1]([O:8][C:9]([NH:11][CH2:12][C:13]1[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[C:15]([OH:21])[CH:14]=1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br[CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25].C(=O)([O-])[O-].[K+].[K+]>CC(=O)CC>[CH2:1]([O:8][C:9]([NH:11][CH2:12][C:13]1[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[C:15]([O:21][CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH:14]=1)=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 11219914benzyl N-[(3-hydroxy-4-methoxyphenyl)methyl]carbamate

생성물 1

HCID 19689412HCID 19689412, 화합물수율 68.6%

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

A mixture comprising 20 g of N-benzyloxycarbonyl-3-hydroxy-4-methoxybenzylamine, 17.43 g of ethyl bromoacetate, 14.43 g of potassium carbonate and 200 ml of 2-butanone, was refluxed under heating with stirring overnight. The mixture was cooled to room temperature. Then, inorganic substances were filtered off, and the filtrate was distilled under reduced pressure. The obtained residue was extracted with chloroform, and the organic layer was washed with water and a saturated sodium chloride aqueous solution and then dried over anhydrous sodium sulfate. Then, the solvent was distilled off. The obtained residue was crystallized from diethyl ether/n-hexane to obtain 17.83 g of the above-identified compound as white crystals.

후처리

  1. temperaturewas refluxed
  2. temperatureunder heating
  3. filtrationThen, inorganic substances were filtered off
  4. distillationthe filtrate was distilled under reduced pressure
  5. extractionThe obtained residue was extracted with chloroform
  6. washthe organic layer was washed with water
  7. dry with materiala saturated sodium chloride aqueous solution and then dried over anhydrous sodium sulfate
  8. distillationThen, the solvent was distilled off
  9. customThe obtained residue was crystallized from diethyl ether/n-hexane

출처 및 근거

ORD 기록
ord-82286defef4b486fb96abf1739796345
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05929074

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