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Water → HCID 22321558、化合物

HRID 496551
ノート
印刷プレビュー

反応式

HRID 496551 の反応式
[N+](=[CH:3][C:4]([C:6]1[CH:10]=[C:9]([CH3:11])[O:8][N:7]=1)=[O:5])=[N-].FC(F)(F)C(O)=[O:15].O>C(OCC)C>[OH:15][CH2:3][C:4]([C:6]1[CH:10]=[C:9]([CH3:11])[O:8][N:7]=1)=[O:5]
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 962WaterHCID 6422Trifluoroacetic acidHCID 73882386HCID 73882386、化合物

生成物 1

HCID 22321558HCID 22321558、化合物収率 61%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

2-Diazo-1-(5-methylisoxazol-3-yl)ethanone (7.0 g, 46 mmol) was dissolved in diethyl ether (100 ml) and trifluoroacetic acid (25 ml) and water (100 ml) were added. The solution was stirred at room temperature for 2 hours, then the diethyl ether was removed in vacuo and the aqueous solution was stirred at room temperature for 18 hours. Further water (100 ml) was added and the aqueous solution was extracted twice with ethyl acetate. The organic extracts were washed successively with water, 10% aqueous potassium carbonate solution and brine, and dried (Na2SO4). Evaporation of the solvent yielded the title-compound as a pale solid (4.0 g, 61%), 1H NMR (360 MHz, CDCl3) 2.52 (3H, s), 4.90 (2H, s), 6.44 (1H, s).

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. customthe diethyl ether was removed in vacuo
  2. stirringthe aqueous solution was stirred at room temperature for 18 hours
  3. additionFurther water (100 ml) was added
  4. extractionthe aqueous solution was extracted twice with ethyl acetate
  5. washThe organic extracts were washed successively with water, 10% aqueous potassium carbonate solution and brine
  6. dry with materialdried (Na2SO4)
  7. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-d342fd922f664990a433ca57590d5266
出典データセット
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06946461B2

反応ノート

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