叠氮化钠 → 4-(AZIDOMETHYL)BENZONITRILE SOLUTION

HRID 855笔记

反应方程式

HRID 855 反应方程式
[N-:1]=[N+:2]=[N-:3].[Na+].[C:5]([C:7]1[CH:14]=[CH:13][C:10]([CH2:11]Br)=[CH:9][CH:8]=1)#[N:6]>O.CN(C=O)C.C1(C)C=CC=CC=1>[C:5]([C:7]1[CH:14]=[CH:13][C:10]([CH2:11][N:1]=[N+:2]=[N-:3])=[CH:9][CH:8]=1)#[N:6]

参与物

6

反应物 2

HCID 33557叠氮化钠HCID 869964-氰基溴苄

产物 1

HCID 110736914-(AZIDOMETHYL)BENZONITRILE SOLUTION

试剂、催化剂与溶剂 3

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂HCID 1140甲苯溶剂HCID 6228N,N-二甲基甲酰胺溶剂

实验过程

A solution of 20.23 g (0.31 mol) sodium azide in 50 ml water was added to 49.15 g (251 mmol) 4-cyanobenzyl bromide in 200 ml DMF at ambient temperature. An exothermic reaction took place and after 1.5 h the reaction mixture was diluted with 200 ml toluene(caution: In order to avoid separation of potentially explosive azide compounds it is adviceable to add the toluene to the reaction mixture before addition of the water) and 500 ml water. The aqueous phase was extracted with an additional 2×50 ml toluene. The combined organic extracts were washed with 2×50 ml water and brine and finally dried (MgSO4) and filtered. The solution was used as such in the next step.

后处理

  1. customAn exothermic reaction
  2. customseparation of potentially explosive azide compounds it
  3. additionto add the toluene to the reaction mixture
  4. additionbefore addition of the water) and 500 ml water
  5. extractionThe aqueous phase was extracted with an additional 2×50 ml toluene
  6. washThe combined organic extracts were washed with 2×50 ml water and brine
  7. dry with materialfinally dried (MgSO4)
  8. filtrationfiltered

来源与证据

ORD记录
ord-a4b47970bbbd496493b0100b353ff70e
来源数据集
uspto-grants-1998_03
专利号
US05723444

反应笔记

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