Formaldehyde → 9,10-Anthracenedione, 1-amino-2-chloro-4-hydroxy-

HRID 542393

반응식

HRID 542393 반응식
[OH2:1].S(=O)(=O)(O)O.C=O.[NH2:9][C:10]1[C:23]2[C:22](=[O:24])[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[C:15](=[O:25])[C:14]=2[C:13](Cl)=[CH:12][C:11]=1[Cl:27]>O>[NH2:9][C:10]1[C:23]2[C:22](=[O:24])[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[C:15](=[O:25])[C:14]=2[C:13]([OH:1])=[CH:12][C:11]=1[Cl:27]

참가 물질

5

반응물 3

HCID 712FormaldehydeHCID 729109,10-Anthracenedione, 1-amino-2,4-dichloro-HCID 21910475Sulfuric acid hydrate (1:1)

생성물 1

HCID 755909,10-Anthracenedione, 1-amino-2-chloro-4-hydroxy-수율 95%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

A stirred reactor is charged with 184 parts of sulfuric acid monohydrate and 4.8 parts (1 equivalent) of paraformaldehyde are added, with stirring, over about 15 minutes. Stirring is continued until a solution is obtained. This solution is then heated to 60°-65° C. and 46.5 parts of 98% 1-amino-2,4-dichloroanthraquinone are added. The reaction mixture is heated for 1 hour to 110° C. and this temperature is maintained for 3 hours. The mixture is cooled to 100° C. and 870 parts of water are added. The resultant suspension is heated to 90°-95° C. and stirred for 2 hours at this temperature, then cooled and filtered. The filter cake is washed with hot water and the product is dried in vacuo at 80°-90° C., affording 43.3 parts (95% yield) of 1-amino-2-chloro-4-hydroxyanthraquinone. Rf =0.29 (eluant: concentrated formic acid, saturated with 1-bromonaphthalene).

후처리

  1. additionare added
  2. stirringStirring
  3. customis obtained
  4. temperatureThis solution is then heated to 60°-65° C.
  5. temperatureThe reaction mixture is heated for 1 hour to 110° C.
  6. temperaturethis temperature is maintained for 3 hours
  7. stirringstirred for 2 hours at this temperature
  8. temperaturecooled
  9. filtrationfiltered
  10. washThe filter cake is washed with hot water
  11. customthe product is dried in vacuo at 80°-90° C.

출처 및 근거

ORD 기록
ord-6c9e49b6536740b6a68ca3ef82e0330e
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04657707

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