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1,2-Dibromoethane → Ethyl 2,3-dihydropyrazolo[5,1-b]oxazole-6-carboxylate

HRID 1158913
ノート
印刷プレビュー

反応式

HRID 1158913 の反応式
[OH:1][C:2]1[NH:6][N:5]=[C:4]([C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:19][CH2:20]Br>C(#N)C>[CH2:10]([O:9][C:7]([C:4]1[CH:3]=[C:2]2[O:1][CH2:19][CH2:20][N:6]2[N:5]=1)=[O:8])[CH3:11]
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 78391,2-DibromoethaneHCID 11430Potassium CarbonateHCID 178469373HCID 178469373、化合物

生成物 1

HCID 69588863Ethyl 2,3-dihydropyrazolo[5,1-b]oxazole-6-carboxylate収率 43.7%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To the stirred suspension of ethyl 5-hydroxy-1H-pyrazole-3-carboxylate (10.34 g, 0.66 mol) and 36.62 g of potassium carbonate in 500 ml of acetonitrile was added 13.68 g of 1,2-dibromoethane, and refluxed for 16 hours. The reaction mixture was allowed to cool to room temperature, then filtered, the solid was washed with acetonitrile. The filtrate was concentrated to an oil. The residue was dissolved in ethyl acetate and extracted with water. The organic phase was dried over MgSO4 and evaporated to dryness. 5.80 g of the desired product was obtained (48%).

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. temperaturerefluxed for 16 hours
  2. filtrationfiltered
  3. washthe solid was washed with acetonitrile
  4. concentrationThe filtrate was concentrated to an oil
  5. dissolutionThe residue was dissolved in ethyl acetate
  6. extractionextracted with water
  7. dry with materialThe organic phase was dried over MgSO4
  8. customevaporated to dryness

出典と根拠

ORDレコード
ord-5ee310285d6143f3a08e8bff9d8ef5fb
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07812014B2

反応ノート

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