Hydrogen Bromide → 4-(Bromoacetyl)pyridine hydrobromide

HRID 4344

反応式

HRID 4344 の反応式
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]

参加物

4

反応物 2

HCID 260Hydrogen BromideHCID 142824-Acetylpyridine

生成物 1

HCID 27762394-(Bromoacetyl)pyridine hydrobromide

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fa8318595eb54ee98aceafd5c8548e7b
出典データセット
uspto-grants-1988_02
特許番号
US04725606

関連ノート

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