Hydrochloric Acid → HCID 12248299, 화합물

HRID 1518952노트

반응식

HRID 1518952 반응식
[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]

참가 물질

3

반응물 2

HCID 313Hydrochloric AcidHCID 198784-tert-Butylpyridine

생성물 1

HCID 12248299HCID 12248299, 화합물수율 104.7%

반응 조건

온도
22 °C

실험 절차

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).

후처리

  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.)

출처 및 근거

ORD 기록
ord-82d522197c6348e1aa34d8143bd5d96d
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09073856B2

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