Sodium hydride → 1-tert-Butyl-3-[7-(3-tert-butylureido)-6-o-tolyl-pyrido[2,3-d]pyrimidin-2-yl]urea

HRID 3409

반응식

HRID 3409 반응식
[NH2:1][C:2]1[N:3]=[CH:4][C:5]2[CH:11]=[C:10]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[CH3:18])[C:9]([NH2:19])=[N:8][C:6]=2[N:7]=1.[H-].[Na+].[C:22]([N:26]=[C:27]=[O:28])([CH3:25])([CH3:24])[CH3:23]>CN(C)C=O>[C:22]([NH:26][C:27]([NH:1][C:2]1[N:3]=[CH:4][C:5]2[CH:11]=[C:10]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[CH3:18])[C:9]([NH:19][C:27]([NH:26][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:28])=[N:8][C:6]=2[N:7]=1)=[O:28])([CH3:25])([CH3:24])[CH3:23]

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 62412tert-Butyl isocyanateHCID 218500312,7-Diamino-6-o-tolyl-pyrido[2,3-d]pyrimidine

생성물 1

HCID 154345561-tert-Butyl-3-[7-(3-tert-butylureido)-6-o-tolyl-pyrido[2,3-d]pyrimidin-2-yl]urea

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A suspension of 0.5 g of 2,7-diamino-6-o-tolyl-pyrido[2,3-d]pyrimidine, prepared as described above in Example 1, in 10 mL of dimethylformamide is reacted with 0.16 g of 60% sodium hydride and stirred at ambient temperature for 1.5 hours. To the suspension is added 0.49 mL of t-butylisocyanate and the mixture stirred overnight at ambient temperature. The reaction mixture is filtered to remove insoluble salts and the filtrate evaporated under reduced pressure. The residue is diluted with water, the insoluble crude product collected by filtration and dried in vacuo. Crystallization from a hexane:ethyl acetate: dichloromethane mixture (3:2:5 v/v/v) afforded the title compound, mp 209°-212° C. dec.

후처리

  1. customprepared
  2. stirringthe mixture stirred overnight at ambient temperature
  3. filtrationThe reaction mixture is filtered
  4. customto remove insoluble salts
  5. customthe filtrate evaporated under reduced pressure
  6. additionThe residue is diluted with water
  7. filtrationthe insoluble crude product collected by filtration
  8. customdried in vacuo
  9. customCrystallization from a hexane

출처 및 근거

ORD 기록
ord-8859698c10bb4c7b910c576bf44215d1
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733913

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