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

HRID 986386노트

반응식

HRID 986386 반응식
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

참가 물질

5

반응물 2

HCID 11430Potassium CarbonateHCID 14032941HCID 14032941, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6569Methyl Ethyl Ketone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c3f4f0b9ac544bca8fd260158c94a46c
출처 데이터셋
uspto-grants-1987_12
특허 번호
US04713381

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