Hydrochloric Acid → HCID 12248299、化合物

HRID 1518952ノート

反応式

HRID 1518952 の反応式
[ClH:1].[C:2]([C:6]1[CH:11]=[CH:10][N:9]=[CH:8][CH:7]=1)([CH3:5])([CH3:4])[CH3:3]>>[ClH:1].[C:2]([C:6]1[CH:11]=[CH:10][N:9]=[CH:8][CH:7]=1)([CH3:5])([CH3:4])[CH3:3]

参加物

3

反応物 2

HCID 313Hydrochloric AcidHCID 198784-tert-Butylpyridine

生成物 1

HCID 12248299HCID 12248299、化合物収率 104.7%

反応条件

温度
22 °C

実験手順

Add a solution of hydrogen chloride (4M in dioxane, 794.36 mmol, 198.59 mL) to 4-tert-butylpyridine (100 mL, 662 mmol) at 22° C. over 30 minutes. The internal temperature rises to 32° C.; control the exotherm with an ice-water bath and the by adjusting rate of the addition. Stir the mixture at 22° C. for one hour and concentrate. Wash the walls of the flask with EtOH. Dry the resulting solid under vacuum (1 mbar, 23-40° C.) to give the title compound as a white solid (119 g, 99%). MS (m/z): 136 (M-HCl+1).

後処理

  1. customrises to 32° C.
  2. customcontrol the exotherm with an ice-water bath and the by adjusting
  3. additionrate of the addition
  4. concentrationconcentrate
  5. washWash the walls of the flask with EtOH
  6. customDry the resulting solid under vacuum (1 mbar, 23-40° C.)

出典と根拠

ORDレコード
ord-82d522197c6348e1aa34d8143bd5d96d
出典データセット
uspto-grants-2015_07
特許番号
US09073856B2

反応ノート

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