Potassium Carbonate → 4H-1,3,4-Oxadiazin-5(6H)-one, 2-(2,6-dimethylimidazo(1,2-a)pyridin-3-yl)-

HRID 986386ノート

反応式

HRID 986386 の反応式
Cl[CH2:2][C:3]([NH:5][NH:6][C:7]([C:9]1[N:13]2[CH:14]=[C:15]([CH3:18])[CH:16]=[CH:17][C:12]2=[N:11][C:10]=1[CH3:19])=[O:8])=[O:4].C(=O)([O-])[O-].[K+].[K+]>C(C(C)=O)C.CN(C)C=O>[CH3:19][C:10]1[N:11]=[C:12]2[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][N:13]2[C:9]=1[C:7]1[O:8][CH2:2][C:3](=[O:4])[NH:5][N:6]=1

参加物

5

反応物 2

HCID 11430Potassium CarbonateHCID 14032941HCID 14032941、化合物

生成物 1

HCID 30653094H-1,3,4-Oxadiazin-5(6H)-one, 2-(2,6-dimethylimidazo(1,2-a)pyridin-3-yl)-収率 16.4%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6569Methyl Ethyl Ketone溶媒

実験手順

A mixture of 21 g of N'-chloroacetyl-2,6-dimethylimidazo[1,2-a]pyridine-3-carbohydrazide and 30 g of potassium carbonate in 200 ml of methyl ethyl ketone and 100 ml of dimethylformamide is stirred with refluxing for 5 hours. After insoluble substances are filtered off, the solvent is distilled off and water is added to the resultant residue. The precipitated crystals are collected by filtration and recrystallized from methanol to give 3 g of 2-(2,6-dimethylimidazo[1,2-a]pyridin-3-yl)-4,6-dihydro-1,3,4-oxadiazin-5-one as white crystals, melting at 313° C. with decomposition.

後処理

  1. temperaturewith refluxing for 5 hours
  2. filtrationAfter insoluble substances are filtered off
  3. distillationthe solvent is distilled off
  4. additionwater is added to the resultant residue
  5. filtrationThe precipitated crystals are collected by filtration
  6. customrecrystallized from methanol

出典と根拠

ORDレコード
ord-c3f4f0b9ac544bca8fd260158c94a46c
出典データセット
uspto-grants-1987_12
特許番号
US04713381

反応ノート

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