Heptane → HCID 58399779、化合物

HRID 537660

反応式

HRID 537660 の反応式
[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

参加物

8

反応物 4

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

生成物 1

HCID 58399779HCID 58399779、化合物収率 88%

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-7e95338f771b4a278185053804772dc4
出典データセット
uspto-grants-2014_10
特許番号
US08865321B2

関連ノート

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