Methane → HCID 86740607、化合物

HRID 1285179ノート

反応式

HRID 1285179 の反応式
[N:1]1([C:12](=[O:13])[C:11]2[N:10]([CH2:14][C:15](=[N:17][OH:18])[NH2:16])[CH:9]=[N:8][C:7]=2[N:5]([CH3:6])[C:3]1=[O:4])[CH3:2].[CH3:19][O-].[Na+].[N:22]1([C:33](=[O:34])[C:32]2[N:31]([CH2:35]C(Cl)=O)[CH:30]=[N:29][C:28]=2[N:26]([CH3:27])[C:24]1=[O:25])[CH3:23].C>CN(C)C=O>[N:1]1([C:12](=[O:13])[C:11]2[N:10]([CH2:14][CH:15]3[N:16]=[C:35]([N:31]4[C:32]5[C:33](=[O:34])[N:22]([CH3:23])[C:24](=[O:25])[N:26]([CH3:27])[C:28]=5[N:29]=[CH:30]4)[O:18][N:17]3[CH3:19])[CH:9]=[N:8][C:7]=2[N:5]([CH3:6])[C:3]1=[O:4])[CH3:2]

参加物

6

反応物 4

HCID 297MethaneHCID 30161851,2,3,6-Tetrahydro-1,3-dimethyl-2,6-dioxo-7H-purine-7-acetyl chlorideHCID 30574902-(Theophyllin-7-yl)-acetamidoximeHCID 10942334Sodium Methoxide

生成物 1

HCID 86740607HCID 86740607、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

5.04 g. of 2-(theophyllin-7-yl)-acetamidoxime and 1.08 g. of sodium methylate are suspended in 60 cm3 dimethylformamide whereafter a solution of 5.13 g. of theophyllin-7-yl-acetyl chloride in 25 cm3 of dimethyl-formamide is added dropwise within 15 minutes. The mixture is heated for 1 hour and after adding a small amount of activated charcoal it is filtered while hot and the filtrate is evaporated at reduced pressure. The residue is dissolved in 100 cm3 0.1N sodium hydrogen carbonate solution while hot and after cooling the crystals are filtered by suction, washed with water and crystallized from 50% aqueous ethanol. Thus 6.6 g. of 3-(theophyllin-7-yl-methyl)-5-(theophylline-7-yl)-methyl-1,2,4-oxadiazole are obtained, m.p.: 271°-272° C.

後処理

  1. temperatureThe mixture is heated for 1 hour
  2. filtrationis filtered while hot and the filtrate
  3. customis evaporated at reduced pressure
  4. dissolutionThe residue is dissolved in 100 cm3 0.1N sodium hydrogen carbonate solution while hot and
  5. temperatureafter cooling the crystals
  6. filtrationare filtered by suction
  7. washwashed with water
  8. customcrystallized from 50% aqueous ethanol

出典と根拠

ORDレコード
ord-5d06331c63064c7a8648c89ff3742de7
出典データセット
uspto-grants-1986_01
特許番号
US04565817

反応ノート

読み込み中…