Sodium Iodide → HCID 67599459, 화합물

HRID 582547

반응식

HRID 582547 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 67599459HCID 67599459, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f8a076c500ce4ebcb8ed728ba249b303
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05925644

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