5,6-dichloropyridine-3-carbonyl Chloride → 3-t-Butyl-5-(5,6-dichloro-3-pyridyl)-1,2,4-oxadiazole

HRID 368284ノート

反応式

HRID 368284 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:9](Cl)=[O:10])[CH:5]=[N:6][C:7]=1[Cl:8].O[NH:13][C:14](=[NH:19])[C:15]([CH3:18])([CH3:17])[CH3:16]>C1(C)C=CC=CC=1>[C:15]([C:14]1[N:19]=[C:9]([C:4]2[CH:5]=[N:6][C:7]([Cl:8])=[C:2]([Cl:1])[CH:3]=2)[O:10][N:13]=1)([CH3:18])([CH3:17])[CH3:16]

参加物

4

反応物 2

HCID 27821565,6-dichloropyridine-3-carbonyl ChlorideHCID 178446865HCID 178446865、化合物

生成物 1

HCID 232882723-t-Butyl-5-(5,6-dichloro-3-pyridyl)-1,2,4-oxadiazole収率 56%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 5,6-dichloro-pyridine-3-carbonyl chloride (1.8 g, 8.6 mmol) and N-hydroxy-2,2-dimethylpropanimidamide (1.0 g, 8.6 mmol) in toluene (40 mL) was stirred at room temperature for two hours and then heated under reflux for four hours. The mixture was cooled to room temperature and filtered through celite, the solids being washed with toluene (20 mL). Evaporation of the combined filtrates under reduced pressure gave the desired product (1.3 g, 56%) as a clear oil which crystallised on standing to a white solid, MP 98-101° C.

後処理

  1. temperatureheated
  2. temperatureunder reflux for four hours
  3. temperatureThe mixture was cooled to room temperature
  4. filtrationfiltered through celite
  5. washthe solids being washed with toluene (20 mL)
  6. customEvaporation of the combined filtrates under reduced pressure

出典と根拠

ORDレコード
ord-a91589b60f7c45e6ae0ca46b4c1d3979
出典データセット
uspto-grants-2000_10
特許番号
US06133294

反応ノート

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