HRID2086233

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID10340

Carbonic acid sodium salt (1:2)

CNa2O3

HCID10635129

6-Chloro-2-Naphthylsulfonyl Chloride

C10H6Cl2O2S

HCID69545931

未命名化合物

PRODUCTS

生成物

结构：CC(C)(C)OC(=O)N1CCC(NN2CCN(S(=O)(=O)c3ccc4cc(Cl)ccc4c3)CC2=O)CC1

HCID69545631

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID8857

Ethyl acetate

C4H8O2

PROCEDURE

实验过程

A solution of the resultant 1-[1-(tert-butoxycarbonyl)-4-piperidinylamino]-2-piperazinone in ethyl acetate (30 ml) and a 10% aqueous solution of sodium carbonate (30 ml) was combined at 0° C. with 6-chloronaphthalene-2-sulfonyl chloride (2.24 g) and stirred at room temperature for 30 minutes, and then the organic phase was separated, washed with brine, dried and concentrated. The residue thus obtained was purified by a column chromatography on a silica gel (hexane:ethyl acetate=1:2) to obtain 1-[1-(tert-Butoxycarbonyl)-4-piperidinylamino]-4-(6-chloronaphthalene-2-sulfonyl)-2-piperazinone (3.55 g) as a colorless amorphous material.

WORKUP

后处理

customthe organic phase was separated
washwashed with brine
customdried
concentrationconcentrated
customThe residue thus obtained
customwas purified by a column chromatography on a silica gel (hexane:ethyl acetate=1:2)

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-8f99910822204a77a931c07b751824dc
来源数据集: uspto-grants-2004_04
DOI: 10.6084/m9.figshare.5104873.v1
专利: US06723722B1
来源说明: uspto-grants-2004_04

反应 SMILES

[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([NH:14][N:15]2[CH2:20][CH2:19][NH:18][CH2:17][C:16]2=[O:21])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C(=O)([O-])[O-].[Na+].[Na+].[Cl:28][C:29]1[CH:30]=[C:31]2[C:36](=[CH:37][CH:38]=1)[CH:35]=[C:34]([S:39](Cl)(=[O:41])=[O:40])[CH:33]=[CH:32]2>C(OCC)(=O)C>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][CH:11]([NH:14][N:15]2[CH2:20][CH2:19][N:18]([S:39]([C:34]3[CH:33]=[CH:32][C:31]4[C:36](=[CH:37][CH:38]=[C:29]([Cl:28])[CH:30]=4)[CH:35]=3)(=[O:40])=[O:41])[CH2:17][C:16]2=[O:21])[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]