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Ethanol → HCID 178523948, 화합물

HRID 1876778
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HRID 1876778 반응식
[CH2:1]([NH2:4])[CH2:2][NH2:3].[F:5][C:6]([F:15])([F:14])[C:7]1[O:11][C:10]([CH2:12]Cl)=[N:9][N:8]=1.C(O)C>CO>[NH:3]1[CH2:2][CH2:1][NH:4][CH2:12]/[C:10]/1=[N:9]/[NH:8][C:7](=[O:11])[C:6]([F:15])([F:14])[F:5]
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참가 물질

5

반응물 3

HCID 702EthanolHCID 3301EthylenediamineHCID 104424452-(Chloromethyl)-5-(trifluoromethyl)-1,3,4-oxadiazole

생성물 1

HCID 178523948HCID 178523948, 화합물수율 46.8%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
-20 °C

실험 절차

The solution of ethylene diamine (89 g) in methanol (305 mL) is stirred and cooled to −20° C. over about 45 minutes. 5-(trifluoromethyl)-2-(chloromethyl)-1,3,4-oxadiazole (79 g) is added slowly to the solution over 90 minutes at −20° C. The resulting slurry is stirred for about 90 minutes at −20° C. Ethanol (482 mL) is added and the slurry is warmed to −5° C. After stirring for about 2 hours at −5° C., the solid is filtered, washed with ethanol (79 mL) and dried at about 55° C. to afford the title compound. (Yield: 46.8%)

후처리

  1. temperaturethe slurry is warmed to −5° C
  2. stirringAfter stirring for about 2 hours at −5° C.
  3. filtrationthe solid is filtered
  4. washwashed with ethanol (79 mL)
  5. customdried at about 55° C.

출처 및 근거

ORD 기록
ord-260bf0b95fb448188e21e99e1230ade0
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08309724B2

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