Potassium Carbonate → Ethyl 2-[4-(cyanomethoxy)phenyl]-2-ethoxycarbonylacetate

HRID 361891ノート

反応式

HRID 361891 の反応式
[CH2:1]([O:3][C:4]([CH:6]([C:12]1[CH:17]=[CH:16][C:15]([OH:18])=[CH:14][CH:13]=1)[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5])[CH3:2].Br[CH2:20][C:21]#[N:22].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[C:21]([CH2:20][O:18][C:15]1[CH:14]=[CH:13][C:12]([CH:6]([C:7]([O:9][CH2:10][CH3:11])=[O:8])[C:4]([O:3][CH2:1][CH3:2])=[O:5])=[CH:17][CH:16]=1)#[N:22]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 11534BromoacetonitrileHCID 12965552HCID 12965552、化合物

生成物 1

HCID 21844455Ethyl 2-[4-(cyanomethoxy)phenyl]-2-ethoxycarbonylacetate収率 84.3%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To 150 ml of acetone were added 14.58 g of ethyl 2-ethoxycarbonyl-2-(4-hydroxyphenyl)acetate, 8.8 g of bromoacetonitrile and 9.6 g of anhydrous potassium carbonate. After refluxing under heating for 5 hours, insoluble materials were removed by filtration, and the resulting filtrate was concentrated to dryness. The residue thus obtained was purified by silica gel column chromatography using toluene as an elution solvent, thereby obtaining 14.2 g of ethyl 2-[4-(cyanomethoxy)phenyl]-2-ethoxycarbonylacetate in the form of colorless oil.

後処理

  1. temperatureAfter refluxing
  2. temperatureunder heating for 5 hours
  3. custominsoluble materials were removed by filtration
  4. concentrationthe resulting filtrate was concentrated to dryness
  5. customThe residue thus obtained
  6. customwas purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-e8cf79690e43414581fa192c1aacb525
出典データセット
uspto-grants-1999_02
特許番号
US05866577

反応ノート

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