Phosphorus oxychloride → 3-benzyl-6-chloro-1H-pyrimidine-2,4-dione

HRID 357129

反応式

HRID 357129 の反応式
P(Cl)(Cl)([Cl:3])=O.[CH2:6]([N:13]1[C:18](=[O:19])[CH2:17][C:16](=O)[NH:15][C:14]1=[O:21])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>C(O)C>[CH2:6]([N:13]1[C:18](=[O:19])[CH:17]=[C:16]([Cl:3])[NH:15][C:14]1=[O:21])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

参加物

4

反応物 2

HCID 24813Phosphorus oxychlorideHCID 2687261-benzylpyrimidine-2,4,6(1H,3H,5H)-trione

生成物 1

HCID 9379413-benzyl-6-chloro-1H-pyrimidine-2,4-dione

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To 16.8 ml of 50% ethanol, 78.7 ml (844 mmol) of phosphorus oxychloride was added dropwise, with stirring under ice cooling conditions. To this solution, 20.62 g (94.5 mmol) of 3-benzylpyrimidine-2,4,6(1H,3H)-trione was added portionwise. This mixture was stirred at 50° C. for 30 minutes and then at 100° C. for 90 minutes. After cooling, the reaction mixture was poured into ice water and stirred for 1 hour. The resulting precipitate was collected by filtration, washed with water and n-hexane and dried to yield 20.12 g (90.0%, white crystal) of the desired product.

後処理

  1. stirringThis mixture was stirred at 50° C. for 30 minutes
  2. temperatureAfter cooling
  3. stirringstirred for 1 hour
  4. filtrationThe resulting precipitate was collected by filtration
  5. washwashed with water and n-hexane
  6. customdried

出典と根拠

ORDレコード
ord-2c562c39279840cabc2aa67d9d7ca4d3
出典データセット
uspto-grants-1998_11
特許番号
US05840732

関連ノート

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