HRID1838867

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID70297

Benzenecarboperoxoic acid, 3-chloro-

C7H5ClO3

结构：CSc1nccc(-c2c(-c3ccc(F)cc3)c(=O)n(C)n2C2CCN(C(=O)OC(C)(C)C)CC2)n1

HCID11698972

未命名化合物

HCID23665763

Sodium Bisulfite

HNaO3S

PRODUCTS

生成物

结构：Cn1c(=O)c(-c2ccc(F)cc2)c(-c2ccnc(S(C)(=O)=O)n2)n1C1CCN(C(=O)OC(C)(C)C)CC1

HCID60061131

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID6212

Chloroform

CHCl3

PROCEDURE

实验过程

To a solution of 4-[4-(4-fluorophenyl)-2-methyl-5-(2-methylsulfanyl-pyrimidin-4-yl)-3-oxo-2,3-dihydro-pyrazol-1-yl]-piperidine-1 carboxylic acid tert-butyl ester, 11, (5.9 g, 12 mmol) in CHCl3 (200 mL) at 0° C. is added meta-chloroperbenzoic acid (4 g, 23.37 mmol). After stirring for 5 minutes, saturated sodium bisulfite (20 mL) is added and the reaction mixture stirred for an additional 5 minutes. The aqueous phase is extracted three times with CH2Cl2, the combined organic phases washed with saturated sodium bicarbonate, dried (MgSO4), filtered and concentrated in vacuo. The crude material is used without further purification.

WORKUP

后处理

stirringthe reaction mixture stirred for an additional 5 minutes
extractionThe aqueous phase is extracted three times with CH2Cl2
washthe combined organic phases washed with saturated sodium bicarbonate
dry with materialdried (MgSO4)
filtrationfiltered
concentrationconcentrated in vacuo
customThe crude material is used without further purification

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-73366fa6ac374c59ad8452392cd8e0be
来源数据集: uspto-grants-2004_01
DOI: 10.6084/m9.figshare.5104873.v1
专利: US06677337B2
来源说明: uspto-grants-2004_01

反应 SMILES

[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([N:14]2[C:18]([C:19]3[CH:24]=[CH:23][N:22]=[C:21](SC)[N:20]=3)=[C:17]([C:27]3[CH:32]=[CH:31][C:30]([F:33])=[CH:29][CH:28]=3)[C:16](=[O:34])[N:15]2[CH3:35])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].Cl[C:37]1C=CC=C(C(OO)=O)C=1.[S:47](=[O:50])(O)[O-:48].[Na+]>C(Cl)(Cl)Cl>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([N:14]2[C:18]([C:19]3[CH:24]=[CH:23][N:22]=[C:21]([S:47]([CH3:37])(=[O:50])=[O:48])[N:20]=3)=[C:17]([C:27]3[CH:28]=[CH:29][C:30]([F:33])=[CH:31][CH:32]=3)[C:16](=[O:34])[N:15]2[CH3:35])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]