HRID68178

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID1140

Toluene

C7H8

HCID78587

Allyl p-toluenesulphonate

C10H12O3S

结构：Cc1cc(NCCCN(C)CCCNc2ccc([N+](=O)[O-])c(C)c2)ccc1[N+](=O)[O-]

HCID86731947

未命名化合物

PRODUCTS

生成物

结构：C=CC[N+](C)(CCCNc1ccc([N+](=O)[O-])c(C)c1)CCCNc1ccc([N+](=O)[O-])c(C)c1.Cc1ccc(S(=O)(=O)[O-])cc1

HCID86731945

未命名化合物

PROCEDURE

实验过程

N1-Methyl-N3-(3-methyl-4-nitrophenyl)-N1-{3-[(3-methyl-4-nitrophenyl)amino]propyl}-1,3-propanediamine (60.2 g, 0.14 mol) from step 7.1 was heated under reflux with allyl p-toluene sulfonate (34.0 g, 0.16 mol) in 500 ml toluene for 6 hours. As the reaction progressed the product separated out in the form of an oily substance. This oil was separated from the supernatant liquid by decanting and dried. On further cooling the oil initially solidified to a glassy material and after drying could be crushed to afford the product as a brown powder. Yield: 66.0 g (72.5%).

WORKUP

后处理

customseparated out in the form of an oily substance
customThis oil was separated from the supernatant liquid
customby decanting
customdried
temperatureOn further cooling the oil
customafter drying could
custombe crushed

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-36d795d1da95405ea6c75daa91c54980
来源数据集: uspto-grants-2014_09
DOI: 10.6084/m9.figshare.5104873.v1
专利: US08821592B1
来源说明: uspto-grants-2014_09

反应 SMILES

[CH3:1][N:2]([CH2:17][CH2:18][CH2:19][NH:20][C:21]1[CH:26]=[CH:25][C:24]([N+:27]([O-:29])=[O:28])=[C:23]([CH3:30])[CH:22]=1)[CH2:3][CH2:4][CH2:5][NH:6][C:7]1[CH:12]=[CH:11][C:10]([N+:13]([O-:15])=[O:14])=[C:9]([CH3:16])[CH:8]=1.[C:31]1([CH3:44])[CH:36]=[CH:35][C:34]([S:37]([O:40]CC=C)(=[O:39])=[O:38])=[CH:33][CH:32]=1.[C:45]1(C)C=CC=C[CH:46]=1>>[C:31]1([CH3:44])[CH:32]=[CH:33][C:34]([S:37]([O-:40])(=[O:38])=[O:39])=[CH:35][CH:36]=1.[CH2:1]([N+:2]([CH3:31])([CH2:3][CH2:4][CH2:5][NH:6][C:7]1[CH:12]=[CH:11][C:10]([N+:13]([O-:15])=[O:14])=[C:9]([CH3:16])[CH:8]=1)[CH2:17][CH2:18][CH2:19][NH:20][C:21]1[CH:26]=[CH:25][C:24]([N+:27]([O-:29])=[O:28])=[C:23]([CH3:30])[CH:22]=1)[CH:45]=[CH2:46]