HRID345996

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID11430

Potassium Carbonate

CK2O3

HCID14797

Potassium hydroxide

HKO

HCID14549312

1-(4-Hydroxy-2,2,6,6-tetramethylpiperidin-1-yl)ethan-1-one

C11H21NO2

结构：CC1(C)CC(Oc2nc(Cl)nc(N3C(C)(C)CCCC3(C)C)n2)CC(C)(C)N1O

HCID19991796

未命名化合物

2 次

PRODUCTS

生成物

结构：CC(=O)N1C(C)(C)CC(Oc2nc(OC3CC(C)(C)N(O)C(C)(C)C3)nc(N3C(C)(C)CCCC3(C)C)n2)CC1(C)C

HCID19991782

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

结构：CCCC[N+](CCCC)(CCCC)CCCC.O=S(=O)([O-])O

催化剂HCID94433

未命名化合物

溶剂HCID962

Water

H2O

溶剂HCID1140

Toluene

C7H8

PROCEDURE

实验过程

4 g of 2-chloro-4-(1-hydroxyl-2,2,6,6-tetramethylpiperidin-4-oxy)-6-(2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine (product from Example 36) are dissolved in 30 ml of toluene, after which 2.6 g of pulverized KOH, 1 g of potassium carbonate and 0.15 g of tetrabutylammonium hydrogen sulfate are added. 1.95 g of 1-acetyl-2,2,6,6-tetramethyl-4-hydroxypiperidine are added with stirring. The mixture is warmed to 60° for 17 hours. After cooling, 30 ml of water are added. The phases are separated. The organic phase is dried over Na2SO4 and evaporated. After recrystalling from methylene chloride/hexane, dissolving the product in hexane/acetic acid and chromatographic purification on an SiO2 column, the above product, which melts at 175°-176°, is obtained.

WORKUP

后处理

temperatureThe mixture is warmed to 60° for 17 hours
temperatureAfter cooling
customThe phases are separated
dry with materialThe organic phase is dried over Na2SO4
customevaporated
dissolutiondissolving the product in hexane/acetic acid
customchromatographic purification on an SiO2 column
customthe above product, which melts at 175°-176°, is obtained

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-2de703f90ef243378d4f1d60e919c3a2
来源数据集: uspto-grants-1991_10
DOI: 10.6084/m9.figshare.5104873.v1
专利: US05059689
来源说明: uspto-grants-1991_10

反应 SMILES

Cl[C:2]1[N:7]=[C:6]([O:8][CH:9]2[CH2:14][C:13]([CH3:16])([CH3:15])[N:12]([OH:17])[C:11]([CH3:19])([CH3:18])[CH2:10]2)[N:5]=[C:4]([N:20]2[C:25]([CH3:27])([CH3:26])[CH2:24][CH2:23][CH2:22][C:21]2([CH3:29])[CH3:28])[N:3]=1.[OH-].[K+].C(=O)([O-])[O-].[K+].[K+].[C:38]([N:41]1[C:46]([CH3:48])([CH3:47])[CH2:45][CH:44]([OH:49])[CH2:43][C:42]1([CH3:51])[CH3:50])(=[O:40])[CH3:39]>C1(C)C=CC=CC=1.S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.O>[C:38]([N:41]1[C:42]([CH3:51])([CH3:50])[CH2:43][CH:44]([O:49][C:2]2[N:7]=[C:6]([O:8][CH:9]3[CH2:14][C:13]([CH3:16])([CH3:15])[N:12]([OH:17])[C:11]([CH3:19])([CH3:18])[CH2:10]3)[N:5]=[C:4]([N:20]3[C:25]([CH3:27])([CH3:26])[CH2:24][CH2:23][CH2:22][C:21]3([CH3:29])[CH3:28])[N:3]=2)[CH2:45][C:46]1([CH3:48])[CH3:47])(=[O:40])[CH3:39]