Ammonia → Bis(4-octoxycarbonylaminocyclohexyl)methane

HRID 615272

반응식

HRID 615272 반응식
[CH2:1]1[CH:6]([CH2:7][CH:8]2[CH2:13][CH2:12][CH:11]([NH2:14])[CH2:10][CH2:9]2)[CH2:5][CH2:4][CH:3]([NH2:15])[CH2:2]1.[C:16](=[O:27])([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])N.N>>[CH2:19]([O:18][C:16]([NH:15][CH:3]1[CH2:2][CH2:1][CH:6]([CH2:7][CH:8]2[CH2:13][CH2:12][CH:11]([NH:14][C:16]([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])=[O:27])[CH2:10][CH2:9]2)[CH2:5][CH2:4]1)=[O:27])[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26]

참가 물질

4

반응물 3

HCID 222AmmoniaHCID 156604,4'-DiaminodicyclohexylmethaneHCID 16240Carbamic acid, octyl ester

생성물 1

HCID 20429700Bis(4-octoxycarbonylaminocyclohexyl)methane

반응 조건

온도
100 °C

실험 절차

Agitated in a reaction vessel are 210 parts of 4,4'-diaminodicyclohexylmethane with 360 parts of O-octyl carbamate and 150 parts of n-octanol-(1) at a reflux temperature of 185° C.-205° C. for 2 hours while the ammonia is removed by means of distillation. At this point, an additional 650 parts of n-octanol are allowed to flow into the reaction mixture and the reaction is continued at reflux temperature for 10 hours. The reaction mixture, which has been cooled to 100° C., is filtered, and the product is allowed to crystallize by cooling the filtrate. By filtration, washing with octanol and drying, 468 parts of bis(4-octoxycarbonylaminocyclohexyl)methane, C31H58N2O4 (molecular weight 522) are obtained corresponding with 89.6 percent theory relative to 4,4'-bisaminodicyclohexylmethane. The melting point is 129° C.-130° C.

후처리

  1. customat a reflux temperature of 185° C.-205° C.
  2. customfor 2 hours
  3. customis removed by means of distillation
  4. temperatureat reflux temperature for 10 hours
  5. filtrationis filtered
  6. customto crystallize
  7. temperatureby cooling the filtrate
  8. filtrationBy filtration
  9. washwashing with octanol
  10. customdrying

출처 및 근거

ORD 기록
ord-67ea79eddd204a538f2800a67b2c474a
출처 데이터셋
uspto-grants-1985_02
특허 번호
US04497963

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