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

HRID 905524

反応式

HRID 905524 の反応式
[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]

参加物

4

反応物 2

HCID 95824,4'-DifluorobenzophenoneHCID 136115-Aminouracil

生成物 1

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

試薬・触媒・溶媒 1

HCID 22921433N-methylpyrrolidone N-cyclohexylpyrrolidone溶媒

反応条件

温度
180 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-314ea98ef5c84e3f9777b506754f39c3
出典データセット
uspto-grants-2011_09
特許番号
US08012541B2

関連ノート

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