Hydrogen Bromide → 4-(Bromoacetyl)pyridine hydrobromide

HRID 4344

반응식

HRID 4344 반응식
C1C=C[NH+]=CC=1.[Br:7][Br-]Br.[BrH:10].[C:11]([C:14]1[CH:19]=[CH:18][N:17]=[CH:16][CH:15]=1)(=[O:13])[CH3:12]>C(O)(=O)C>[BrH:7].[Br:10][CH2:12][C:11]([C:14]1[CH:19]=[CH:18][N:17]=[CH:16][CH:15]=1)=[O:13]

참가 물질

4

반응물 2

HCID 260Hydrogen BromideHCID 142824-Acetylpyridine

생성물 1

HCID 27762394-(Bromoacetyl)pyridine hydrobromide

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

A twelve-liter three neck flask fitted with an efficient mechanical stirrer, 250 mL dropping funnel, and internal thermometer was charged with glacial acetic acid (5000 mL), pyridinium bromide perbromide (90%, 830 g, 2.60 mol) and 30% hydrobromic acid in acetic acid (525 mL). After stirring at room temperature for ninety minutes, 4-acetylpyridine (250 g, 2.07 mol) was added dropwise over forty-five minutes. Upon completion of the addition the reaction mixture was cooled with an ice bath to 15° C. and the product, which had precipitated, was collected by filtration, washed with ether and air-dried. The crude α-bromo-4-acetylpyridine hydrobromide (566.3 g, 97%) was sufficiently pure for subsequent reactions, mp. 177.5°-182.0° C.

후처리

  1. customA twelve-liter three neck flask fitted with an efficient mechanical stirrer
  2. additionUpon completion of the addition the reaction mixture
  3. temperaturewas cooled with an ice bath to 15° C.
  4. customthe product, which had precipitated
  5. filtrationwas collected by filtration
  6. washwashed with ether
  7. customair-dried

출처 및 근거

ORD 기록
ord-fa8318595eb54ee98aceafd5c8548e7b
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04725606

연결된 노트

불러오는 중…