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Ammonia → HCID 21472906, 화합물

HRID 981598
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HRID 981598 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

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

생성물 1

HCID 21472906HCID 21472906, 화합물

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9d6bb02d1e594ac8b2d371e07fc626b7
출처 데이터셋
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04992473

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