海萝胶 → 4-氯代苯酐

HRID 1109823

反应方程式

HRID 1109823 反应方程式
Cl[C:2]1[C:3]([O:5][C:6](=[O:8])[CH:7]=1)=[O:4].[Cl:9][C:10]1=[C:11](Cl)[C:12](O[C:15]1=O)=O.C1C2NC3C(=CC=CC=3)SC=2C=CC=1.C=CC(Cl)=C.Cl>O>[Cl:9][C:10]1[CH:15]=[C:7]2[C:6](=[O:8])[O:5][C:3](=[O:4])[C:2]2=[CH:12][CH:11]=1

参与物

7

反应物 5

HCID 313海萝胶HCID 7108吩噻嗪HCID 313692-氯-1,3-丁二烯HCID 66772CHLOROMALEIC ACID ANHYDRIDEHCID 707282,3-二氯马来酸酐

产物 1

HCID 670444-氯代苯酐收率 80%

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

反应条件

温度
105 °C

实验过程

A 3-necked 50 mL flask was equipped with a pressure equalizing addition funnel, a thermocouple well with thermocouple, a water cooled condensor and a magnetic stir bar. The flask was charged with 13.2 g (0.10 mol) of a 90/10 GC area % mixture of monochloromaleic anhydride and dichloromaleic anhydride and 100 mg of phenothiazine and 0.5 g of activated carbon. The contents of the flask were heated to 80 to 130° C. and 8.8 g (0.1 mol) of chloroprene was added over 15 to 30 minutes. HCl gas was observed evolving from the reactor. After 6 hours at 130° C. the contents of the flask were sparged with oxygen for 2 hours between 130° and 150° C., filtered hot, and multiple distilled into two fractions resulting in the isolation of 13.2 g (80% of theoretical) of 4-chlorophthalic anhydride.

后处理

  1. customA 3-necked 50 mL flask was equipped with a pressure
  2. additionaddition funnel
  3. customAfter 6 hours at 130° C. the contents of the flask were sparged with oxygen for 2 hours between 130° and 150° C.
  4. filtrationfiltered hot
  5. distillationmultiple distilled into two fractions

来源与证据

ORD记录
ord-c5705182af3645479a36841d24a96591
来源数据集
uspto-grants-1994_06
专利号
US05322954

关联笔记

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