四氯化碳 → Benzene, 1-methyl-3-(trichloromethyl)-

HRID 1981680

反应方程式

HRID 1981680 反应方程式
[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][CH:10]=1)[CH:5]([Cl:7])[Cl:6].[OH-].[Na+].C(Cl)(Cl)(Cl)[Cl:14]>CCCCCCCCCCCC[N+](C)(C)C.[Cl-]>[CH3:1][C:2]1[CH:3]=[C:4]([C:5]([Cl:14])([Cl:7])[Cl:6])[CH:8]=[CH:9][CH:10]=1

参与物

5

反应物 3

HCID 5943四氯化碳HCID 14798二甲基对苯二胺二盐酸HCID 587420间甲基二氯苄

产物 1

HCID 599554Benzene, 1-methyl-3-(trichloromethyl)-收率 101.3%

试剂、催化剂与溶剂 1

HCID 8152十二烷基三甲基氯化铵催化剂

实验过程

70.0 gms of 3-methyl benzal chloride dissolved in 286.4 gms of carbon tetrachloride was charged into a reaction vessel with 2.67 gms of Aliquat 4 (dodecyltrimethylammonium chloride in alcohol). 192 gms of 50% aqueous sodium hydroxide was added and the mixture heated to reflux for a period of about 4 hours. During this period water was continuously removed from the reaction media using a Dean Stark Trap. After completion of the reaction, the mixture was filtered, water was added to the mixture, and the organic layer was separated by phase separation. The organic layer was stripped on a rotary evaporator to give 84.9 gms of a clear yellow oil. (Yield 93.4%).

后处理

  1. temperaturethe mixture heated
  2. temperatureto reflux for a period of about 4 hours
  3. customDuring this period water was continuously removed from the reaction media
  4. customAfter completion of the reaction
  5. filtrationthe mixture was filtered
  6. additionwater was added to the mixture
  7. customthe organic layer was separated by phase separation
  8. customThe organic layer was stripped on a rotary evaporator

来源与证据

ORD记录
ord-ccd16b13fb7842e7813ae4946baa47b7
来源数据集
uspto-grants-1986_06
专利号
US04593144

关联笔记

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