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Dicyclohexylcarbodiimide → Diisopropyl ether ethanol

HRID 1939891
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HRID 1939891 반응식
[OH:1][C:2]1[C:10]2N=NNC=2C=C[CH:3]=1.[CH:11]1(N=C=NC2CCCCC2)[CH2:16]CCC[CH2:12]1>CN(C)C=O>[CH2:2]([OH:1])[CH3:3].[CH:11]([O:1][CH:2]([CH3:3])[CH3:10])([CH3:16])[CH3:12]
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참가 물질

4

반응물 2

HCID 10868DicyclohexylcarbodiimideHCID 178418300HCID 178418300, 화합물

생성물 1

HCID 23358034Diisopropyl ether ethanol

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
5 °C

실험 절차

Then, at 20° C., 18.3 g (0.12 mol) of hydroxybenzotriazole (HOBT), 23.7 g (0.109 mol) of N-4-trifluoromethylbenzyl-N-n-propylamine and 25.6 g (0.125 mol) of dicyclohexyl-carbodiimide (DCCI) and a further 250 ml of dimethylformamide (DMF) were added. The mixture was left to react for 24 hours. It was then cooled to 5° C. and filtered. 500 ml of water were added to the filtrate and it was extracted with ethyl acetate. The combined organic phases were washed with water and saturated sodium hydrogen carbonate solution, dried with magnesium sulphate and filtered over kieselguhr/char-coal. After working up in the usual way, 50 g of colourless crystals of the title compound are obtained by crystallisation from ethanol/diisopropylether (1:1). The 3H-PAF-receptor bonding--determined using human thrombocytes--is Ki =1.8 nMol/liter. (The method used is described for example in European Patent Application 368 175).

후처리

  1. waitThe mixture was left
  2. customto react for 24 hours
  3. filtrationfiltered
  4. addition500 ml of water were added to the filtrate and it
  5. extractionwas extracted with ethyl acetate
  6. washThe combined organic phases were washed with water and saturated sodium hydrogen carbonate solution
  7. dry with materialdried with magnesium sulphate
  8. filtrationfiltered over kieselguhr/char-coal

출처 및 근거

ORD 기록
ord-ca2cdcfad3ee4f1285418e0b70278f44
출처 데이터셋
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05698552

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