HRID2059105

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID5565

N1,N2-Bis(2-aminoethyl)-1,2-ethanediamine

C6H18N4

HCID14798

Sodium Hydroxide

HNaO

结构：CC1(C)CC(C(O)CNc2nc(Cl)nc(NCC(O)C3CC(C)(C)NC(C)(C)C3)n2)CC(C)(C)N1

HCID86738304

未命名化合物

PRODUCTS

生成物

结构：CC1(C)CC(C(O)CNc2nc(NCCN(CCN(CCNc3nc(NCC(O)C4CC(C)(C)NC(C)(C)C4)nc(NCC(O)C4CC(C)(C)NC(C)(C)C4)n3)c3nc(NCC(O)C4CC(C)(C)NC(C)(C)C4)nc(NCC(O)C4CC(C)(C)NC(C)(C)C4)n3)c3nc(NCC(O)C4CC(C)(C)NC(C)(C)C4)nc(NCC(O)C4CC(C)(C)NC(C)(C)C4)n3)nc(NCC(O)C3CC(C)(C)NC(C)(C)C3)n2)CC(C)(C)N1

HCID86738307

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID962

Water

H2O

溶剂HCID31275

1,4-Dioxane

C4H8O2

PROCEDURE

实验过程

2,4-Bis{2-hydroxy-N-(2,2,6,6-tetramethyl-4-piperidyl)ethylamino}-6-chloro-1,3,5-triazine (8.0 g) and triethylenetetramine (0.5 g) were dissolved in dioxane (100 ml) and to the solution was added an aqueous solution of sodium hydroxide (0.7 g) in water (10 ml). The mixture was heated to reflux for 6 hours. Dioxane was distilled off from the reaction mixture and the residue was extracted with benzene. The extract was treated with silica gel column chromatography (eluent=ethyl acetate:benzene:ethanol:triethylamine=20:4:2:1) to give the desired product as white crystals melting at 158° C.

WORKUP

后处理

temperatureThe mixture was heated
temperatureto reflux for 6 hours
distillationDioxane was distilled off from the reaction mixture
extractionthe residue was extracted with benzene
additionThe extract was treated with silica gel column chromatography (eluent=ethyl acetate:benzene:ethanol:triethylamine=20:4:2:1)

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-b27f0edc11d948079e1ba986925693d5
来源数据集: uspto-grants-1982_03
DOI: 10.6084/m9.figshare.5104873.v1
专利: US04321374
来源说明: uspto-grants-1982_03

反应 SMILES

[OH:1][CH:2]([CH:26]1[CH2:31][C:30]([CH3:33])([CH3:32])[NH:29][C:28]([CH3:35])([CH3:34])[CH2:27]1)[CH2:3][NH:4][C:5]1[N:10]=[C:9]([NH:11][CH2:12][CH:13]([CH:15]2[CH2:20][C:19]([CH3:22])([CH3:21])[NH:18][C:17]([CH3:24])([CH3:23])[CH2:16]2)[OH:14])[N:8]=[C:7](Cl)[N:6]=1.[NH2:36][CH2:37][CH2:38][NH:39][CH2:40][CH2:41][NH:42][CH2:43][CH2:44][NH2:45].[OH-:46].[Na+]>O1CCOCC1.O>[OH:1][CH:2]([CH:26]1[CH2:31][C:30]([CH3:33])([CH3:32])[NH:29][C:28]([CH3:35])([CH3:34])[CH2:27]1)[CH2:3][NH:4][C:5]1[N:10]=[C:9]([NH:11][CH2:12][CH:13]([CH:15]2[CH2:20][C:19]([CH3:22])([CH3:21])[NH:18][C:17]([CH3:24])([CH3:23])[CH2:16]2)[OH:14])[N:8]=[C:7]([NH:36][CH2:37][CH2:38][N:39]([C:7]2[N:8]=[C:9]([NH:11][CH2:12][CH:13]([CH:15]3[CH2:16][C:17]([CH3:24])([CH3:23])[NH:18][C:19]([CH3:21])([CH3:22])[CH2:20]3)[OH:14])[N:10]=[C:5]([NH:4][CH2:3][CH:2]([CH:26]3[CH2:27][C:28]([CH3:35])([CH3:34])[NH:29][C:30]([CH3:33])([CH3:32])[CH2:31]3)[OH:1])[N:6]=2)[CH2:40][CH2:41][N:42]([C:7]2[N:8]=[C:9]([NH:11][CH2:12][CH:13]([CH:15]3[CH2:16][C:17]([CH3:24])([CH3:23])[NH:18][C:19]([CH3:21])([CH3:22])[CH2:20]3)[OH:14])[N:10]=[C:5]([NH:4][CH2:3][CH:2]([CH:26]3[CH2:27][C:28]([CH3:35])([CH3:34])[NH:29][C:30]([CH3:33])([CH3:32])[CH2:31]3)[OH:1])[N:6]=2)[CH2:43][CH2:44][NH:45][C:7]2[N:8]=[C:9]([NH:11][CH2:12][CH:13]([CH:15]3[CH2:20][C:19]([CH3:22])([CH3:21])[NH:18][C:17]([CH3:23])([CH3:24])[CH2:16]3)[OH:46])[N:10]=[C:5]([NH:4][CH2:3][CH:2]([CH:26]3[CH2:27][C:28]([CH3:35])([CH3:34])[NH:29][C:30]([CH3:33])([CH3:32])[CH2:31]3)[OH:1])[N:6]=2)[N:6]=1