Phosgene → 2-Biphenylylsulfonylisocyanate

HRID 615530

반응식

HRID 615530 반응식
[C:1]1([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[S:7]([NH2:10])(=[O:9])=[O:8].C(N=[C:22]=[O:23])CCC.N12CCN(CC1)CC2.C(Cl)(Cl)=O>ClC1C=CC=CC=1>[C:1]1([C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[S:7]([N:10]=[C:22]=[O:23])(=[O:9])=[O:8]

참가 물질

6

반응물 4

HCID 6371Phosgene3회HCID 8110Butyl isocyanateHCID 9237DabcoHCID 123715202-Phenylbenzene-1-sulfonamide

생성물 1

HCID 131033202-Biphenylylsulfonylisocyanate

시약·촉매·용매 1

HCID 7964Chlorobenzene용매

실험 절차

23.3 g of 2-biphenylylsulfonamide, 10.9. g of n-butyl isocyanate, a catalytic amount of 1,4-diazabicyclo[2,2,2]-octane and 180 ml of chlorobenzene were refluxed with stirring for 2 hours. Then, phosgene in a slight excess of the theroretical amount was blown through the reaction mixture over 2 hours while maintaining the internal temperature at 115°-120° C. At this time, any unreacted phosgene escaping from the reaction system was trapped in a dry ice trap and returned to the reactor. After addition of the phosgene, the reaction mixture was further stirred at the reflux temperature for a short time to complete the reaction. The mixture was cooled, and if necessary, it was filtered under reduced pressure to remove the insoluble matter. It was then concentrated under reduced pressure, to obtain 20.0 g of 2-biphenylylsulfonylisocyanate. B.p. 135°-137° C./0.7-0.8 mmHg.

후처리

  1. temperaturewhile maintaining the internal temperature at 115°-120° C
  2. stirringthe reaction mixture was further stirred at the reflux temperature for a short time
  3. customthe reaction
  4. temperatureThe mixture was cooled
  5. filtrationif necessary, it was filtered under reduced pressure
  6. customto remove the insoluble matter
  7. concentrationIt was then concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-35c9e98dc0e14b8ea55cba1d7f3e5a81
출처 데이터셋
uspto-grants-1985_02
특허 번호
US04500342

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