4,4'-Difluorobenzophenone → N-(5-uracil-yl)-4,4'-difluorobenzophenone imine

HRID 1911799

반응식

HRID 1911799 반응식
[NH2:1][C:2]1[C:3](=[O:9])[NH:4][C:5](=[O:8])[NH:6][CH:7]=1.[F:10][C:11]1[CH:25]=[CH:24][C:14]([C:15]([C:17]2[CH:22]=[CH:21][C:20]([F:23])=[CH:19][CH:18]=2)=O)=[CH:13][CH:12]=1>CN1CCCC1=O.C1(N2CCCC2=O)CCCCC1>[NH:6]1[CH:7]=[C:2]([N:1]=[C:15]([C:14]2[CH:24]=[CH:25][C:11]([F:10])=[CH:12][CH:13]=2)[C:17]2[CH:18]=[CH:19][C:20]([F:23])=[CH:21][CH:22]=2)[C:3](=[O:9])[NH:4][C:5]1=[O:8]

참가 물질

4

반응물 2

HCID 95824,4'-DifluorobenzophenoneHCID 136115-Aminouracil

생성물 1

HCID 59595635N-(5-uracil-yl)-4,4'-difluorobenzophenone imine

시약·촉매·용매 1

HCID 22921433N-methylpyrrolidone N-cyclohexylpyrrolidone용매

반응 조건

온도
180 °C

실험 절차

In a round bottom flask equipped with an overhead stirrer, 1.16 grams (0.009 mole) of 5-aminouracil was charged along with 6 grams (0.027 mole) of 4,4′-difluorobenzophenone and a N-methylpyrrolidone/N-cyclohexylpyrrolidone solvent mixture (50/50, 20 milliliters). The reaction mixture was then heated to 180° C. for 3 days. A charge of hexanes (100 milliliters) was added to fully induce precipitation, and the solid was isolated by filtration and twice recrystallized from isopropanol. The product was rinsed with isopropanol, suction dried, and vacuum dried in an oven overnight.

후처리

  1. customIn a round bottom flask equipped with an overhead stirrer
  2. additionwas added to fully induce precipitation
  3. customthe solid was isolated by filtration
  4. customtwice recrystallized from isopropanol
  5. washThe product was rinsed with isopropanol, suction
  6. customdried
  7. customvacuum dried in an oven overnight

출처 및 근거

ORD 기록
ord-44cd58c4353b4c54a50e189ea613d1de
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08604135B2

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