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

HRID 3409ノート

反応式

HRID 3409 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8859698c10bb4c7b910c576bf44215d1
出典データセット
uspto-grants-1998_03
特許番号
US05733913

反応ノート

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