Dimethyl Sulfoxide → N-(Hexahydro-1,5-dimethyl-2,4,6-trioxo-5-pyrimidinyl)-2,3,4,5-tetrafluorobenzamide

HRID 1097278ノート

反応式

HRID 1097278 の反応式
Cl.[NH2:2][C:3]1([CH3:13])[C:8](=[O:9])[N:7]([CH3:10])[C:6](=[O:11])[NH:5][C:4]1=[O:12].[F:14][C:15]1[C:16]([F:28])=[C:17]([F:27])[C:18]([F:26])=[C:19]2C(=O)O[C:21](=[O:22])[C:20]=12.CCN(CC)CC.CS(C)=O>O>[CH3:10][N:7]1[C:8](=[O:9])[C:3]([NH:2][C:21](=[O:22])[C:20]2[CH:19]=[C:18]([F:26])[C:17]([F:27])=[C:16]([F:28])[C:15]=2[F:14])([CH3:13])[C:4](=[O:12])[NH:5][C:6]1=[O:11]

参加物

6

反応物 4

HCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 69545Tetrafluorophthalic anhydrideHCID 66811031HCID 66811031、化合物

生成物 1

HCID 24765565N-(Hexahydro-1,5-dimethyl-2,4,6-trioxo-5-pyrimidinyl)-2,3,4,5-tetrafluorobenzamide

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
153 °C

実験手順

A mixture of 5-amino-1,5-dimethylbarbituric acid hydrochloride (0.42 g, 2 mmol), tetrafluorophthalic anhydride (0.44 g, 2 mmol), Et3N (0.28 mL, 0.20 g, 2 mmol) and DMSO (3 mL) was stirred and heated at 153° C. for 5 hours. The reaction mixture was then allowed to cool down to room temperature and poured into water (10 mL). The oil that immediately formed was carefully removed from the solution, from which a solid precipitated after 4 days standing at room temperature. The precipitate was collected by filtration, washed with water and dried under reduced pressure to give 20a as yellow crystals.

後処理

  1. temperatureto cool down to room temperature
  2. customThe oil that immediately formed
  3. customwas carefully removed from the solution, from which a solid
  4. customprecipitated after 4 days
  5. customstanding at room temperature
  6. filtrationThe precipitate was collected by filtration
  7. washwashed with water
  8. customdried under reduced pressure

出典と根拠

ORDレコード
ord-63e15b5ce3de44278155a60744c3de3c
出典データセット
uspto-grants-2012_03
特許番号
US08143252B2

反応ノート

読み込み中…