Propylamine → HCID 86682303、化合物

HRID 1055199ノート

反応式

HRID 1055199 の反応式
[CH2:1]([NH2:4])[CH2:2][CH3:3].[F:5][CH:6]([C:12]([CH3:14])=[O:13])[C:7]([O:9]CC)=O>>[F:5][CH:6]([C:12](=[O:13])[CH3:14])[C:7]([NH:4][CH2:1][CH2:2][CH3:3])=[O:9]

参加物

3

反応物 2

HCID 7852PropylamineHCID 230078Ethyl 2-fluoroacetoacetate

生成物 1

HCID 86682303HCID 86682303、化合物

実験手順

0.8 mol (65.8 ml) of n-propylamine were added dropwise within 0.5 h to 0.2 mol (25 ml) of ethyl 2-fluoroacetoacetat. The reaction mixture was heated and then held for 2 h at 60° C. Then it was evaporated to dryness, dissolved in 50 ml water and 60 ml ethanol and adjusted with 32% HCl to pH 3. It was again evaporated, dissolved in 300 ml ethyl acetate, filtered and again evaporated to dryness. 17 g of crude product was chromatographed over 800 g silica gel with ethyl acetate/hexane 1/1. After drying, 14 g of the title compound were obtained.

後処理

  1. temperatureThe reaction mixture was heated
  2. customThen it was evaporated to dryness
  3. dissolutiondissolved in 50 ml water
  4. customIt was again evaporated
  5. dissolutiondissolved in 300 ml ethyl acetate
  6. filtrationfiltered
  7. customagain evaporated to dryness
  8. custom17 g of crude product was chromatographed over 800 g silica gel with ethyl acetate/hexane 1/1
  9. customAfter drying

出典と根拠

ORDレコード
ord-eb119db03f7445929edcb5ad0a7f695d
出典データセット
uspto-grants-2016_07
特許番号
US09394324B2

反応ノート

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