醋酸 → 2,3,4-Tribromo-5-(chloromethyl)thiophene

HRID 127758

反应方程式

HRID 127758 反应方程式
C=O.[ClH:3].[Br:4][C:5]1[C:9]([Br:10])=[C:8]([Br:11])[S:7][CH:6]=1.[C:12](O)(=O)C>>[Cl:3][CH2:12][C:6]1[S:7][C:8]([Br:11])=[C:9]([Br:10])[C:5]=1[Br:4]

参与物

5

反应物 4

HCID 176醋酸HCID 313海萝胶HCID 712多聚甲醛2 次HCID 765932,3,4-三溴噻吩

产物 1

HCID 151249082,3,4-Tribromo-5-(chloromethyl)thiophene

反应条件

温度
70 °C

实验过程

4.07 G. (50 mmol) of formalin (37%) and 40 ml. of concentrated hydrochloric acid were added to a solution of 10.2 g. (33.3 mmol) of 3,4,5-tribromothiophene in 20 ml. of acetic acid. The resulting mixture was warmed to 70° C. After 6 hrs., 4.07 g. of formalin were added and heating was continued overnight. The resulting mixture was cooled, poured on ice water and extracted with ether. The organic phase was washed twice with water, sodium bicarbonate and water, dried and evaporated to give crude 2-chloromethyl-3,4,5-tribromothiophene.

后处理

  1. temperatureheating
  2. waitwas continued overnight
  3. temperatureThe resulting mixture was cooled
  4. additionpoured on ice water
  5. extractionextracted with ether
  6. washThe organic phase was washed twice with water, sodium bicarbonate and water
  7. customdried
  8. customevaporated

来源与证据

ORD记录
ord-9510259a80f744889a12dc20c83a48cf
来源数据集
uspto-grants-1981_03
专利号
US04256878

关联笔记

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