Formaldehyde → Dihydrobenzoxazine

HRID 637623

반응식

HRID 637623 반응식
[CH2:1]=[O:2].[OH-].[K+].[NH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.O[C:13]1C=CC(C(C2C=CC(O)=CC=2)(C)C)=CC=1>C1(C)C=CC=CC=1.CO>[O:2]1[C:1]2[CH:13]=[CH:7][CH:8]=[CH:9][C:10]=2[CH2:11][CH2:6][NH:5]1

참가 물질

7

반응물 4

HCID 712FormaldehydeHCID 6115Aniline2회HCID 6623Bisphenol AHCID 14797Potassium Hydroxide

생성물 1

HCID 21887592Dihydrobenzoxazine

시약·촉매·용매 2

HCID 887Methanol용매HCID 1140Toluene용매

실험 절차

To a reactor are charged 66 parts of paraformaldehyde, 66 parts of methanol and 1 part of potassium hydroxide. The mixture is warmed and stirred until the paraform dissolves. While the temperature is maintained in the 25°-35° C. range, 93 parts of aniline are added to the paraform solution. Upon completion of the aniline addition the reaction is stirred for 15 minutes and then 114 parts of bisphenol A are added. The reaction is heated to atmospheric reflux and refluxed for 1 hour. After 1 hour, toluene (100 parts) is added to the reaction mixture while it is being cooled. A water layer forms which is removed. The toluene is removed by heating and applying reduced pressure until a temperature of 90° C. at 7 kPa pressure is reached. The appropriate solvent is added at this point. The devolitilized resin has a % closed dihydrobenzoxazine ring of 87%, and a calculated equivalent weight of 262.

후처리

  1. temperatureThe mixture is warmed
  2. dissolutiondissolves
  3. additionare added to the paraform solution
  4. stirringis stirred for 15 minutes
  5. temperatureThe reaction is heated
  6. temperatureto atmospheric reflux
  7. temperaturerefluxed for 1 hour
  8. temperatureis being cooled
  9. customA water layer forms which is removed
  10. customThe toluene is removed
  11. temperatureby heating
  12. customuntil a temperature of 90° C.
  13. additionThe appropriate solvent is added at this point
  14. customclosed dihydrobenzoxazine ring of 87%

출처 및 근거

ORD 기록
ord-51ce1ec740604c1cb2be25c6918b2d43
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04557979

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