Methane → HCID 86740607, 화합물

HRID 1285179노트

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HRID 1285179 반응식
[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]

참가 물질

6

반응물 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

생성물 1

HCID 86740607HCID 86740607, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5d06331c63064c7a8648c89ff3742de7
출처 데이터셋
uspto-grants-1986_01
특허 번호
US04565817

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