HRID1109482

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID78205

Carbonochloridic acid, (4-nitrophenyl)methyl ester

C8H6ClNO4

HCID81531

Diisopropylethylamine

C8H19N

结构：Nc1ccc(C(=O)N2CCN(CCc3ccc(Cl)cc3)CC2)cc1

HCID18946357

未命名化合物

PRODUCTS

生成物

结构：O=C(Nc1ccc(C(=O)N2CCN(CCc3ccc(Cl)cc3)CC2)cc1)OCc1ccc([N+](=O)[O-])cc1

HCID19020593

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID8028

Tetrahydrofuran

C4H8O

2 次

PROCEDURE

实验过程

1 g of 1-[4-aminobenzoyl]-4-[2-(4-chlorophenyl)ethyl]-piperazine and 0.4 g of Hunig base (=N-ethyldiisopropylamine) are dissolved in 15 ml of tetrahydrofuran. A solution of 0.75 g of chloroformic acid 4-nitrobenzyl ester in 5 ml of tetrahydrofuran is added dropwise thereto. The reaction solution is stirred for 3.5 hours at room temperature and for 2 hours at a bath temperature of 55°. The solution is concentrated by evaporation and the residue is taken up in methylene chloride and washed with water. Colourless crystals of 1-[4-(N-4-nitrobenzyloxycarbonylamino)benzoyl]-4-[2-(4-chlorophenyl)ethyl]-piperazine having a melting point of 146°-148° are obtained from alcohol.

WORKUP

后处理

concentrationThe solution is concentrated by evaporation
washwashed with water

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-0446c28d2be64a35af886c1a6a40c558
来源数据集: uspto-grants-1994_06
DOI: 10.6084/m9.figshare.5104873.v1
专利: US05321027
来源说明: uspto-grants-1994_06

反应 SMILES

[NH2:1][C:2]1[CH:24]=[CH:23][C:5]([C:6]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][C:16]3[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=3)[CH2:10][CH2:9]2)=[O:7])=[CH:4][CH:3]=1.CCN(C(C)C)C(C)C.[N+:34]([C:37]1[CH:47]=[CH:46][C:40]([CH2:41][O:42][C:43](Cl)=[O:44])=[CH:39][CH:38]=1)([O-:36])=[O:35]>O1CCCC1>[N+:34]([C:37]1[CH:38]=[CH:39][C:40]([CH2:41][O:42][C:43]([NH:1][C:2]2[CH:3]=[CH:4][C:5]([C:6]([N:8]3[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][C:16]4[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=4)[CH2:10][CH2:9]3)=[O:7])=[CH:23][CH:24]=2)=[O:44])=[CH:46][CH:47]=1)([O-:36])=[O:35]