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Ammonia → HCID 21472906、化合物

HRID 981598
ノート
印刷プレビュー

反応式

HRID 981598 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][CH2:16][C:17]([CH3:19])=O)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH3:20].[ClH:21]>C(O)C.[Ni]>[Cl-:21].[CH3:19][CH:17]([NH3+:20])[CH2:16][CH2:15][C:12]1[CH:13]=[CH:14][C:9]([O:8][CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[CH:10][CH:11]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 140103234-(4-Benzyloxyphenyl)butan-2-one

生成物 1

HCID 21472906HCID 21472906、化合物

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

実験手順

A solution of 40.0 g of methyl 2-(4-benzyloxyphenyl)ethyl ketone and 160 ml of anhydrous ammonia in 300 ml of ethanol was heated at 75° C. and stirred for two hours. After cooling the reaction mixture to room temperature, 4.0 g of Raney nickel was added in one portion, and the reaction mixture then was stirred at 25° C. for twelve hours under a hydrogen atmosphere at 300 psi. The reaction mixture next was filtered and the filtrate was concentrated by evaporation of the solvent under reduced pressure to provide an oil. The oil was dissolved in 120 ml of 3N hydrochloric acid, from which the product as a hydrochloride salt precipitated. The salt so formed was collected by filtration and recrystallized from methanol and toluene to provide 36.2 g of dl-1-methyl-3-(4-benzyloxyphenyl)propylaminium chloride. M. P. 195°-197.5° C.

後処理

  1. stirringthe reaction mixture then was stirred at 25° C. for twelve hours under a hydrogen atmosphere at 300 psi
  2. filtrationThe reaction mixture next was filtered
  3. concentrationthe filtrate was concentrated by evaporation of the solvent under reduced pressure
  4. customto provide an oil
  5. customprecipitated
  6. customThe salt so formed
  7. filtrationwas collected by filtration
  8. customrecrystallized from methanol and toluene

出典と根拠

ORDレコード
ord-9d6bb02d1e594ac8b2d371e07fc626b7
出典データセット
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04992473

反応ノート

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