Phosgene → 2-Biphenylylsulfanylisocyanate

HRID 279733

反応式

HRID 279733 の反応式
[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)=O.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:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[S:7][N:10]=[C:22]=[O:23]

参加物

6

反応物 4

HCID 6371Phosgene3 回HCID 8110Butyl isocyanateHCID 9237DabcoHCID 123715202-Phenylbenzene-1-sulfonamide

生成物 1

HCID 233223832-Biphenylylsulfanylisocyanate

試薬・触媒・溶媒 1

HCID 7964Chlorobenzene溶媒

実験手順

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-biphenylylsulfanylisocyanate, B.p 135°-137° C./0.7-0.8 mmHg.

後処理

  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

出典と根拠

ORDレコード
ord-b803ebad71d248dab033f98c2b32ba6c
出典データセット
uspto-grants-1986_05
特許番号
US04586951

関連ノート

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