Acetonitrile → HCID 21438854、化合物

HRID 329162ノート

反応式

HRID 329162 の反応式
CC(C[N:5]1[C:11](=[O:12])O[C:8](=O)[C:7]2=[CH:13][CH:14]=[CH:15][CH:16]=[C:6]12)=O.CS[C:19](=[NH:22])NC.I.[CH3:24]N(C)C(=N)S.C(=O)([O-])[O-].[Na+].[Na+].[C:36](#[N:38])[CH3:37]>>[CH3:37][C:36]1[CH:19]([CH3:24])[N:22]2[C:11](=[O:12])[N:5]=[C:6]3[C:7]([CH:13]=[CH:14][CH:15]=[CH:16]3)=[C:8]2[N:38]=1

参加物

5

反応物 4

HCID 6342AcetonitrileHCID 10340Sodium CarbonateHCID 122260031-(2-oxopropyl)-2,4-dihydro-1H-3,1-benzoxazine-2,4-dioneHCID 178484400HCID 178484400、化合物

生成物 1

HCID 21438854HCID 21438854、化合物

実験手順

A mixture of 11.0 g. of N-methylcarbonylmethyl isatoic anhydride, 16.6 g. of S,N-dimethyl-thiopseudourea -dimethyl-thiopseudourea hydroiodide, 5.5 g. of sodium carbonate and 150 ml. of acetonitrile is refluxed for one-half hour, filtered, evaporated to dryness, the residue dissolved in methylene chloride and evaporated again to dryness. The residue is taken up in diglyme, refluxed for one-half hour and cooled with stirring to obtain a precipitate which is recovered by filtering, washed with ether, dissolved in methylene chloride, treated with carbon, alumina and sodium sulfate, filtered through celite, and the methylene chloride exchanged for ether. The resulting precipitate is recovered by filtering, washed with ether and dried under reduced pressure to obtain 2,3-dimethyl-imidazo[1,2-c]quinazolin-5(3H)-one, m.p. 234°-237° C.

後処理

  1. additionA mixture of 11.0 g
  2. filtrationfiltered
  3. customevaporated to dryness
  4. dissolutionthe residue dissolved in methylene chloride
  5. customevaporated again to dryness
  6. temperaturerefluxed for one-half hour
  7. temperaturecooled
  8. customto obtain a precipitate which
  9. customis recovered
  10. filtrationby filtering
  11. washwashed with ether
  12. dissolutiondissolved in methylene chloride
  13. additiontreated with carbon, alumina and sodium sulfate
  14. filtrationfiltered through celite
  15. customThe resulting precipitate is recovered
  16. filtrationby filtering
  17. washwashed with ether
  18. customdried under reduced pressure

出典と根拠

ORDレコード
ord-02cc006ac98942f2ad1d2d9652b4a004
出典データセット
uspto-grants-1977_04
特許番号
US04020062

反応ノート

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