Heptane → HCID 58399779, 화합물

HRID 537660

반응식

HRID 537660 반응식
[C:1]1([NH:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[NH2:14])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N(C(C)C)C(C)C)C.Cl[C:25]1[N:30]=[C:29]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[N:28]=[C:27]([C:37]2[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=2)[N:26]=1.CCCCCCC>C1COCC1.C(O)C.ClCCl>[C:1]1([NH:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[NH:14][C:25]2[N:30]=[C:29]([C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=3)[N:28]=[C:27]([C:37]3[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=3)[N:26]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

8

반응물 4

HCID 8900HeptaneHCID 196982-Chloro-4,6-diphenyl-1,3,5-triazineHCID 68297N-Phenyl-o-phenylenediamineHCID 81531Diisopropylethylamine

생성물 1

HCID 58399779HCID 58399779, 화합물수율 88%

시약·촉매·용매 3

HCID 702Ethanol용매HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
0 °C

실험 절차

44.3 g (240 mmol) of N-phenyl-o-phenylenediamine are initially introduced in THF and cooled to 0° C., and 136.4 ml (818 mmol) of N-ethyldiisopropylamine are added dropwise. The mixture is subsequently stirred at room temperature for a further 1 h. A solution of 64.4 g (240 mmol) of 2-chloro-4,6-diphenyl-1,3,5-triazine, dissolved in 1600 ml of THF, is then added dropwise, and the mixture is stirred at 60° C. for 96 h. After cooling, the solution is stirred with 400 ml of heptane, 80 ml of dichloromethane and 100 ml of ethanol. The solid is washed with toluene and washed by stirring with hot heptane, giving 87.7 g (211 mmol) of a crystalline solid. The overall yield is 88%.

후처리

  1. additionis then added dropwise
  2. stirringthe mixture is stirred at 60° C. for 96 h
  3. temperatureAfter cooling
  4. washThe solid is washed with toluene
  5. washwashed
  6. stirringby stirring with hot heptane

출처 및 근거

ORD 기록
ord-7e95338f771b4a278185053804772dc4
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08865321B2

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