Ethyl bromoacetate → HCID 19689412、化合物

HRID 583102ノート

反応式

HRID 583102 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 19689412HCID 19689412、化合物収率 68.6%

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-82286defef4b486fb96abf1739796345
出典データセット
uspto-grants-1999_07
特許番号
US05929074

反応ノート

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