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

HRID 2287131
ノート
印刷プレビュー

反応式

HRID 2287131 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-da647925251d4c3babb3fa97faf4f2e9
出典データセット
uspto-grants-1981_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04269788

反応ノート

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