HRID441643

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID4875

Potassium iodide

HCID8082

Piperidine

C5H11N

结构：CCn1c2ccc(C(=O)CCCCl)cc2c2cc(C(=O)CCCCl)ccc21

HCID12331790

1,1'-(9-Ethyl-9H-carbazole-3,6-diyl)bis(4-chlorobutan-1-one)

C22H23Cl2NO2

PRODUCTS

生成物

结构：CCn1c2ccc(C(=O)CCCN3CCCCC3)cc2c2cc(C(=O)CCCN3CCCCC3)ccc21.CCn1c2ccc(C(=O)CCCN3CCCCC3)cc2c2cc(C(=O)CCCN3CCCCC3)ccc21.Cl.Cl.Cl.Cl.O

HCID131710034

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID31275

1,4-Dioxane

C4H8O2

PROCEDURE

实验过程

A mixture of 19.5 g (0.048 mole) of N-ethyl-3,6-bis-(4-chlorobutyryl)carbazole, 34.0 g (0.4 mole) of piperidine and 2.0 g of potassium iodide in 250 ml of p-dioxane is heated at reflux for 68 hours with stirring, then filtered. Upon cooling, the mixture is diluted with 500 ml of water, and the resulting semi-solid is dissolved in ether, washed repeatedly with water and dried over magnesium sulfate. The ethereal solution is treated with etheral HCl to give N-ethyl-3,6-bis(4-piperidinobutyryl)carbazole dihydrochloride hemihydrate, which is recrystallized from methanol-ethyl acetate, M.P. 138°-142° C.

WORKUP

后处理

temperatureis heated
temperatureat reflux for 68 hours
filtrationfiltered
temperatureUpon cooling
additionthe mixture is diluted with 500 ml of water
dissolutionthe resulting semi-solid is dissolved in ether
washwashed repeatedly with water
dry with materialdried over magnesium sulfate
additionThe ethereal solution is treated with etheral HCl

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-0d0111a1023743679181461d6a19bdb3
来源数据集: uspto-grants-1977_08
DOI: 10.6084/m9.figshare.5104873.v1
专利: US04041165
来源说明: uspto-grants-1977_08

反应 SMILES

[CH2:1]([N:3]1[C:15]2[CH:14]=[CH:13][C:12]([C:16](=[O:21])[CH2:17][CH2:18][CH2:19][Cl:20])=[CH:11][C:10]=2[C:9]2[C:4]1=[CH:5][CH:6]=[C:7]([C:22](=[O:27])[CH2:23][CH2:24][CH2:25]Cl)[CH:8]=2)[CH3:2].[NH:28]1[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]1.[I-].[K+]>O1CCOCC1>[OH2:21].[ClH:20].[ClH:20].[CH2:1]([N:3]1[C:15]2[CH:14]=[CH:13][C:12]([C:16](=[O:21])[CH2:17][CH2:18][CH2:19][N:28]3[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]3)=[CH:11][C:10]=2[C:9]2[C:4]1=[CH:5][CH:6]=[C:7]([C:22](=[O:27])[CH2:23][CH2:24][CH2:25][N:28]1[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]1)[CH:8]=2)[CH3:2].[CH2:1]([N:3]1[C:15]2[CH:14]=[CH:13][C:12]([C:16](=[O:21])[CH2:17][CH2:18][CH2:19][N:28]3[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]3)=[CH:11][C:10]=2[C:9]2[C:4]1=[CH:5][CH:6]=[C:7]([C:22](=[O:27])[CH2:23][CH2:24][CH2:25][N:28]1[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]1)[CH:8]=2)[CH3:2].[ClH:20].[ClH:20]