Hydrochloric Acid → 4-Chlorophthalic anhydride

HRID 1109823

반응식

HRID 1109823 반응식
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

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 7108PhenothiazineHCID 31369ChloropreneHCID 66772Chloromaleic anhydrideHCID 70728Dichloromaleic anhydride

생성물 1

HCID 670444-Chlorophthalic anhydride수율 80%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
105 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c5705182af3645479a36841d24a96591
출처 데이터셋
uspto-grants-1994_06
특허 번호
US05322954

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