1-Chloro-2-nitrobenzene → Disulfide, bis(2-nitrophenyl)

HRID 2290971

반응식

HRID 2290971 반응식
Cl[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9].[S-:11][S-:12].[Na+].[Na+]>O>[CH:5]1[CH:4]=[C:3]([N+:8]([O-:10])=[O:9])[C:2]([S:11][S:12][C:2]2[C:3]([N+:8]([O-:10])=[O:9])=[CH:4][CH:5]=[CH:6][CH:7]=2)=[CH:7][CH:6]=1

참가 물질

4

반응물 2

HCID 69451-Chloro-2-nitrobenzene4회HCID 89870Sodium disulfide

생성물 1

HCID 70861Disulfide, bis(2-nitrophenyl)수율 95%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

1300 parts of water containing 150 parts of castor oil ethoxylate and 250 parts of 1-chloro-2-nitrobenzene are charged to a reactor and heated to 60° C. with thorough mixing. Simultaneous addition is then made of 2268 parts of disulfide solution (preparation as described in Example 1) and 2250 parts of 1-chloro-2-nitrobenzene in separate streams. The rate of addition is 400 parts per hour. When the total amount of chloronitrobenzene has been added, the remaining amount of disulfide is added at a rate of 100 parts per hour. The reaction is slightly exothermic and the temperature is kept in the range from 60°-65° C. by cooling. During the reaction, both the continuously added chloronitrobenzene and the resultant disulfide are continuously dispersed in the reaction mixture. This is done by constant and intensive mixing. Agglomerates are comminuted with a dismembrator. After the total amount of disulfide has been added as well, stirring is continued until the reaction mass consists of individual yellow crystals and of a colourless to tea-coloured mother liquor. The batch is then cooled to 40° C. and filtered. The product is washed with cold water until the washings are colourless, affording 2,2'-dinitrodiphenyl disulfide which contains about 5% of by-products. The yield is 95%.

후처리

  1. additionSimultaneous addition
  2. additionThe rate of addition
  3. customis kept in the range from 60°-65° C.
  4. temperatureby cooling
  5. customDuring the reaction
  6. customAgglomerates are comminuted with a dismembrator
  7. temperatureThe batch is then cooled to 40° C.
  8. filtrationfiltered
  9. washThe product is washed with cold water until the washings

출처 및 근거

ORD 기록
ord-ed87e70287f94215bb444d4f45096742
출처 데이터셋
uspto-grants-1986_10
특허 번호
US04618721

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