Propylamine → HCID 86682303, 화합물

HRID 1055199노트

반응식

HRID 1055199 반응식
[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]

참가 물질

3

반응물 2

HCID 7852PropylamineHCID 230078Ethyl 2-fluoroacetoacetate

생성물 1

HCID 86682303HCID 86682303, 화합물

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-eb119db03f7445929edcb5ad0a7f695d
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09394324B2

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