三溴化硼 → 3,4-二羟基-5-碘代苯甲醛

HRID 2571

反应方程式

HRID 2571 反应方程式
[I: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>[I: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 794995-碘香兰素

产物 1

HCID 140282113,4-二羟基-5-碘代苯甲醛收率 66.2%

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 5-iodo vanillin (commercial) and 360 ml of dichloromethane were mixed together under nitrogen and the mixture was cooled to 0° C. 135 ml of a molar solution of boron tribromide in dichloromethane were added and the mixture stood for 16 hours at ambient temperature and was then concentrated, cooled to 0° C. and acidified. The crystallized product was separated out, washed with water, dried and crystallized from an isopropanol--water mixture (1-2 by volume) to obtain 23.4 g of the expected product.

后处理

  1. concentrationwas then concentrated
  2. temperaturecooled to 0° C.
  3. customThe crystallized product was separated out
  4. washwashed with water
  5. customdried
  6. customcrystallized from an isopropanol

来源与证据

ORD记录
ord-23ad7b54403248708606eeee9fbf6470
来源数据集
uspto-grants-1998_03
专利号
US05728828

关联笔记

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