Phenol → Urea Urethane

HRID 1158185

반응식

HRID 1158185 반응식
CC1C=CC([N:8]=[C:9]=[O:10])=CC=1[N:11]=[C:12]=[O:13].C1C([NH2:20])=CC=C(S(C2C=CC(N)=CC=2)(=O)=O)C=1.[C:31]1([OH:37])C=CC=C[CH:32]=1.C(N(CC)CC)C>C(C(C)=O)C>[NH2:20][C:12]([NH2:11])=[O:13].[NH2:8][C:9]([O:37][CH2:31][CH3:32])=[O:10]

참가 물질

6

반응물 4

HCID 996PhenolHCID 2955DapsoneHCID 8471TriethylamineHCID 11443Toluene 2,4-Diisocyanate

생성물 1

HCID 21585015Urea Urethane수율 549.8%

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매4회

반응 조건

온도
30 °C

실험 절차

To 158.5 g of 2,4-toluene diisocyanate was added 240 g of methyl ethyl ketone as a solvent, and 107.5 g of 4,4′-diaminodiphenyl sulfone was added thereto in the form of powder at 30° C. with stirring at 400 rpm over a period of 8 hours. After 1 hour, 26 g of methyl ethyl ketone was added thereto and stirred for another 15 hours to obtain a white viscous slurry reaction mixture. Then, a solution of 89.5 g of phenol in 15.8 g of methyl ethyl ketone was poured into the reaction mixture to be dissolved therein, after which 9.3 g of a 1 wt % solution of triethylamine in methyl ethyl ketone was added thereto as a catalyst over a period of 2 hours, and the reaction was uninterruptedly carried out for 1 hour. Thereafter, the reaction mixture was cooled to 20° C. and continuously stirred for 3 hours to obtain a slurry containing slightly yellow crystals precipitated therein. The slurry was freed of the solvent and concentrated under reduced pressure to be solidified, after which the resulting solid was ground and then dried overnight in a vacuum to obtain 355 g of a urea-urethane composition as slightly yellow powder.

후처리

  1. waitAfter 1 hour
  2. stirringstirred for another 15 hours
  3. customto obtain
  4. customa white viscous slurry reaction mixture
  5. dissolutionto be dissolved
  6. waitas a catalyst over a period of 2 hours
  7. waitthe reaction was uninterruptedly carried out for 1 hour
  8. temperatureThereafter, the reaction mixture was cooled to 20° C.
  9. stirringcontinuously stirred for 3 hours
  10. customto obtain a slurry
  11. additioncontaining slightly yellow crystals
  12. customprecipitated
  13. concentrationconcentrated under reduced pressure
  14. customdried overnight in a vacuum

출처 및 근거

ORD 기록
ord-960d7d6d22e34aa193fc969503faf89e
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07807738B2

연결된 노트

불러오는 중…