三溴化硼 → 3-氯-4,5-二羟基苯甲醛

HRID 2569

反应方程式

HRID 2569 反应方程式
[Cl:1][C:2]1[C:3]([OH:12])=[C:4]([O:10]C)[CH:5]=[C:6]([CH:9]=1)[CH:7]=[O:8].B(Br)(Br)Br>ClCCl>[Cl:1][C:2]1[CH:9]=[C:6]([CH:5]=[C:4]([OH:10])[C:3]=1[OH:12])[CH:7]=[O:8]

参与物

4

反应物 2

HCID 25134三溴化硼HCID 296225-氯香草醛

产物 1

HCID 24681823-氯-4,5-二羟基苯甲醛收率 77.3%

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂2 次

反应条件

温度
0 °C

实验过程

37.2 g of commercial 5-chloro vanillin and 800 ml of dichloromethane were mixed together under nitrogen and cooled to 0° C. 300 ml of a molar solution of boron tribromide in dichloromethane are added and the mixture stood for one night at ambient temperature. It was concentrated, cooled again to 0° C. and acidified. The crystallized product was separated, washed with water, dried and crystallized from an isopropanol- water mixture (1-2 by volume) to obtain 26.6 g of the expected product melting at >260° C.

后处理

  1. waitthe mixture stood for one night at ambient temperature
  2. concentrationIt was concentrated
  3. temperaturecooled again to 0° C.
  4. customThe crystallized product was separated
  5. washwashed with water
  6. customdried
  7. customcrystallized from an isopropanol- water mixture (1-2 by volume)

来源与证据

ORD记录
ord-49d72313e0d6412c95d675c45339c241
来源数据集
uspto-grants-1998_03
专利号
US05728828

关联笔记

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