HRID1761436

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID25681

1-(3-Chlorophenyl)piperazine hydrochloride

C10H14Cl2N2

HCID14280583

未命名化合物

PRODUCTS

生成物

结构：Cl.Cl.O.O=C1CC2(CCCC2)CC(=O)N1OCCCN1CCN(c2cccc(Cl)c2)CC1.O=C1CC2(CCCC2)CC(=O)N1OCCCN1CCN(c2cccc(Cl)c2)CC1

HCID131715732

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID8471

Triethylamine

C6H15N

PROCEDURE

实验过程

A solution of 8-(3-bromopropyloxy)-8-azaspiro[4.5]decan-7,9-dione (4.0 g) and 1-(3-chlorophenyl)piperazine hydrochloride (3.06 g) in 50 ml of Et3N was heated to reflux with stirring under N2. After 1 hour TLC (thin layer chromatography) showed the absence of starting material. The excess Et3N was removed in vacuo and the residue chromatographed on silica using ethyl acetate as the eluent. Fractions containing the desired product were combined and concentrated in vacuo.

WORKUP

后处理

temperatureto reflux
customThe excess Et3N was removed in vacuo
customthe residue chromatographed on silica
additionFractions containing the desired product
concentrationconcentrated in vacuo

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-c55a9c5047b041e78a0ff6d57ab68f58
来源数据集: uspto-grants-1989_05
DOI: 10.6084/m9.figshare.5104873.v1
专利: US04826846
来源说明: uspto-grants-1989_05

反应 SMILES

Br[CH2:2][CH2:3][CH2:4][O:5][N:6]1[C:15](=[O:16])[CH2:14][C:9]2([CH2:13][CH2:12][CH2:11][CH2:10]2)[CH2:8][C:7]1=[O:17].[ClH:18].[Cl:19][C:20]1[CH:21]=[C:22]([N:26]2[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]2)[CH:23]=[CH:24][CH:25]=1>CCN(CC)CC>[OH2:5].[ClH:19].[Cl:19][C:20]1[CH:21]=[C:22]([N:26]2[CH2:31][CH2:30][N:29]([CH2:2][CH2:3][CH2:4][O:5][N:6]3[C:15](=[O:16])[CH2:14][C:9]4([CH2:13][CH2:12][CH2:11][CH2:10]4)[CH2:8][C:7]3=[O:17])[CH2:28][CH2:27]2)[CH:23]=[CH:24][CH:25]=1.[Cl:19][C:20]1[CH:21]=[C:22]([N:26]2[CH2:31][CH2:30][N:29]([CH2:2][CH2:3][CH2:4][O:5][N:6]3[C:15](=[O:16])[CH2:14][C:9]4([CH2:13][CH2:12][CH2:11][CH2:10]4)[CH2:8][C:7]3=[O:17])[CH2:28][CH2:27]2)[CH:23]=[CH:24][CH:25]=1.[ClH:18]