Isobutyryl chloride → 6-Bromo-3-(propan-2-yl)[1,2,4]triazolo[4,3-a]pyridine--hydrogen chloride (1/1)

HRID 498074노트

반응식

HRID 498074 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][NH2:9])=[N:6][CH:7]=1.[C:10]([Cl:15])(=O)[CH:11]([CH3:13])[CH3:12]>CCCCCC>[ClH:15].[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:10]([CH:11]([CH3:13])[CH3:12])=[N:9][N:8]=2)[CH:7]=1

참가 물질

4

반응물 2

HCID 62325Isobutyryl chlorideHCID 115356995-Bromo-2-hydrazinopyridine

생성물 1

HCID 221701776-Bromo-3-(propan-2-yl)[1,2,4]triazolo[4,3-a]pyridine--hydrogen chloride (1/1)

시약·촉매·용매 1

HCID 8058Hexane용매

실험 절차

A 500 ml three-necked round-bottomed flask equipped with a mechanical stirrer and a condenser, connected on top to a nitrogen bubbler and a thermometer, was charged with 5-bromo-pyridin-2-yl-hydrazine (43.4 g, 0.231 moles) and isobutyryl chloride (218 ml, 2.08 moles). The mixture was gently refluxed for 3 hours. The heating source was then replaced with an ice-water bath and the slurry cooled to room temperature. Hexane (220 ml) was added and the slurry stirred at room temperature for 15 minutes and filtered. The cake was washed with hexane (3×70 ml) and then dried in a vacuum-oven (35° C.) for 48 hours. The title compound was obtained as an off-white powder (58.96 g, yield 92.3%).

후처리

  1. customA 500 ml three-necked round-bottomed flask equipped with a mechanical stirrer and a condenser
  2. temperatureThe mixture was gently refluxed for 3 hours
  3. customThe heating source was then replaced with an ice-water bath
  4. filtrationfiltered
  5. washThe cake was washed with hexane (3×70 ml)
  6. customdried in a vacuum-oven (35° C.) for 48 hours

출처 및 근거

ORD 기록
ord-567c3671f56e4df3955f2b4807fa3bd8
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06949652B2

반응 노트

불러오는 중…