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Acetic Anhydride → N-ethyl-N-[1-methyl-2-(1-phenyl-2,5-cyclohexadien-1-yl)ethyl]-acetamide

HRID 2287131
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HRID 2287131 반응식
[CH3:1][CH:2]([NH:16][CH2:17][CH3:18])[CH2:3][C:4]1([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:9]=[CH:8][CH2:7][CH:6]=[CH:5]1.[C:19](OC(=O)C)(=[O:21])[CH3:20].C(=O)(O)[O-].[K+]>N1C=CC=CC=1>[CH2:17]([N:16]([CH:2]([CH3:1])[CH2:3][C:4]1([C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)[CH:5]=[CH:6][CH2:7][CH:8]=[CH:9]1)[C:19](=[O:21])[CH3:20])[CH3:18]
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참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 516893Potassium BicarbonateHCID 23459459alpha-methyl-N-ethyl-1-phenyl-2,5-cyclohexadien-1-ethylamine

생성물 1

HCID 23459464N-ethyl-N-[1-methyl-2-(1-phenyl-2,5-cyclohexadien-1-yl)ethyl]-acetamide

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

1.5 g. of α-methyl-N-ethyl-1-phenyl-2,5-cyclohexadien-1-ethylamine are dissolved in a mixture of 10 ml. of acetic acid anhydride and 8 ml. of pyridine and left to stand at room temperature overnight. Then, the mixture is stirred for 2 hours with 2 N aqueous potassium bicarbonate solution and subsequently extracted with ether. The ether phase is washed with dilute aqueous hydrochloride acid and then with water, dried with sodium sulfate, filtered and concentrated to dryness. The crude product obtained is chromatographed on silica gel with ether. There is obtained N-ethyl-N-[1-methyl-2-(1-phenyl-2,5-cyclohexadien-1-yl)ethyl]-acetamide in the form of an oily product.

후처리

  1. extractionsubsequently extracted with ether
  2. washThe ether phase is washed with dilute aqueous hydrochloride acid
  3. dry with materialwith water, dried with sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated to dryness
  6. customThe crude product obtained
  7. customis chromatographed on silica gel with ether

출처 및 근거

ORD 기록
ord-da647925251d4c3babb3fa97faf4f2e9
출처 데이터셋
uspto-grants-1981_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04269788

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