Sodium Iodide → HCID 67599459、化合物

HRID 582547

反応式

HRID 582547 の反応式
[Br:1][C:2]1[C:3]([NH:10][CH2:11][CH:12]([O:14][C:15]2[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][C:16]=2[CH3:22])[CH3:13])=[N:4][CH:5]=[N:6][C:7]=1[CH2:8][CH3:9].[C:23]([O:31][CH2:32]Cl)(=[O:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.[I-:34].[Na+]>CC(C)=O>[I-:34].[C:23]([O:31][CH2:32][N+:6]1[C:7]([CH2:8][CH3:9])=[C:2]([Br:1])[C:3]([NH:10][CH2:11][CH:12]([O:14][C:15]2[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][C:16]=2[CH3:22])[CH3:13])=[N:4][CH:5]=1)(=[O:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

参加物

5

反応物 3

HCID 5238Sodium IodideHCID 79257Chloromethyl benzoateHCID 537398875-Bromo-6-ethyl-4-[2-(2,4-dimethylphenoxy)-propylamino]pyrimidine

生成物 1

HCID 67599459HCID 67599459、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

0.3 g (8.2 mmol) of 5-bromo-6-ethyl-4-[2-(2,4-dimethylphenoxy)-propylamino]pyrimidine (according to EP-A-57 440), 0.17 g (9.8 mmol) of chloromethyl benzoate and 0.12 g (8.2 mmol) of sodium iodide in 25 ml of acetone were heated under reflux for 8 hours. After cooling, the precipitated sodium chloride was filtered off and the filtrate was concentrated. The residue was taken up in dichloromethane and washed by stirring with water. The organic phase was dried and concentrated. The residue was digested with ethyl acetate. Filtration with suction gave 0.97 g (53.3% of theory) of light-yellow crystals. mp.: 159-161° C.

後処理

  1. temperatureunder reflux for 8 hours
  2. temperatureAfter cooling
  3. filtrationthe precipitated sodium chloride was filtered off
  4. concentrationthe filtrate was concentrated
  5. washwashed
  6. customThe organic phase was dried
  7. concentrationconcentrated
  8. filtrationFiltration with suction
  9. customgave 0.97 g (53.3% of theory) of light-yellow crystals

出典と根拠

ORDレコード
ord-f8a076c500ce4ebcb8ed728ba249b303
出典データセット
uspto-grants-1999_07
特許番号
US05925644

関連ノート

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