Hydrochloric Acid → HCID 21844246、化合物

HRID 1901323ノート

反応式

HRID 1901323 の反応式
C(O)C.[CH2:4]([O:6][C:7]([CH:9]([C:15]1[CH:20]=[CH:19][C:18]([O:21][CH2:22][C:23](OCC)=[NH:24])=[CH:17][CH:16]=1)[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[O:8])[CH3:5].[CH2:28](N)[CH2:29][NH2:30].Cl>O>[CH2:13]([O:12][C:10]([CH:9]([C:15]1[CH:16]=[CH:17][C:18]([O:21][CH2:22][C:23]2[NH:24][CH2:28][CH2:29][N:30]=2)=[CH:19][CH:20]=1)[C:7]([O:6][CH2:4][CH3:5])=[O:8])=[O:11])[CH3:14]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 702Ethanol3 回HCID 3301EthylenediamineHCID 21844471Ethyl 2-ethoxycarbonyl-2-[4-(2-ethoxy-2-iminoethoxy)phenyl)acetate

生成物 1

HCID 21844246HCID 21844246、化合物収率 54.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

With ice cooling and stirring, 40 ml of ethanol solution containing 3.6 g of ethyl 2-ethoxycarbonyl-2-[4-(2-ethoxy-2-iminoethoxy]phenyl]acetate obtained in the above step b) was added dropwise to a 10 ml ethanol solution containing 0.6 g of ethylenediamine, and the resulting mixture was stirred at room temperature for 1.5 hours, followed by refluxing under heating for 0.5 hours. After cooling, the resulting reaction solution was adjusted to an acidic pH with ethanol containing 13% (w/v) of hydrochloric acid, and then concentrated to dryness. The residue thus obtained was dissolved in water and washed with diethyl ether. Thereafter, the resulting water layer was adjusted to pH 9-10 with dilute sodium hydroxide aqueous solution, and crystals thus precipitated were collected by filtration. In this way, 1.83 g of the title compound was obtained in the form of colorless crystals.

後処理

  1. customobtained in the above step b)
  2. stirringthe resulting mixture was stirred at room temperature for 1.5 hours
  3. temperatureby refluxing
  4. temperatureunder heating for 0.5 hours
  5. temperatureAfter cooling
  6. customthe resulting reaction solution
  7. concentrationconcentrated to dryness
  8. customThe residue thus obtained
  9. washwashed with diethyl ether
  10. customthus precipitated
  11. filtrationwere collected by filtration

出典と根拠

ORDレコード
ord-5b6d253c4f264bbcb4a4444b0cfbd2ec
出典データセット
uspto-grants-1996_11
特許番号
US05576343

反応ノート

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