HRID535439

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID6497

Dimethyl sulfate

C2H6O4S

HCID24758

Sodium hydride

HNa

结构：CC(C(=O)Nc1ccc(NC(=O)C2CCOCC2)c(C#Cc2ccccc2)n1)N(C)C(=O)OC(C)(C)C

HCID86694390

未命名化合物

PRODUCTS

生成物

结构：CC(C(=O)Nc1ccc(N(C)C(=O)C2CCOCC2)c(C#Cc2ccccc2)n1)N(C)C(=O)OC(C)(C)C

HCID86694429

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID8028

Tetrahydrofuran

C4H8O

PROCEDURE

实验过程

At RT NaH (60% dispersion in mineral oil, 2.3 mg, 0.0.06 mmol) is added to tert-butyl-N-methyl-N-[1-[[5-(oxane-4-carbonylamino)-6-(2-phenylethynyl)pyridin-2-yl]amino]-1-oxopropan-2-yl]carbamate E5b (35 mg, 0.04 mmol) in THF (1 ml). After stirring for 10 minutes dimethylsulfate (4 μl, 0.06 mmol) is added to the mixture and stirring continued for 20 minutes. The mixture is concentrated in vacuo and the product purified by RP HPLC. Yield: 5 mg (23%). HPLC-MS: M+H=521; tR=2.06 min (*Method—2).

WORKUP

后处理

additionis added to the mixture
concentrationThe mixture is concentrated in vacuo
customthe product purified by RP HPLC

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-c8b67e50d4d14b7a883374dfc0be6981
来源数据集: uspto-grants-2014_10
DOI: 10.6084/m9.figshare.5104873.v1
专利: US08859541B2
来源说明: uspto-grants-2014_10

反应 SMILES

[H-].[Na+].[C:3]([O:7][C:8](=[O:39])[N:9]([CH3:38])[CH:10]([CH3:37])[C:11]([NH:13][C:14]1[CH:19]=[CH:18][C:17]([NH:20][C:21]([CH:23]2[CH2:28][CH2:27][O:26][CH2:25][CH2:24]2)=[O:22])=[C:16]([C:29]#[C:30][C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[N:15]=1)=[O:12])([CH3:6])([CH3:5])[CH3:4].[CH3:40]OS(OC)(=O)=O>C1COCC1>[C:3]([O:7][C:8](=[O:39])[N:9]([CH3:38])[CH:10]([CH3:37])[C:11]([NH:13][C:14]1[CH:19]=[CH:18][C:17]([N:20]([CH3:40])[C:21]([CH:23]2[CH2:24][CH2:25][O:26][CH2:27][CH2:28]2)=[O:22])=[C:16]([C:29]#[C:30][C:31]2[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=2)[N:15]=1)=[O:12])([CH3:5])([CH3:6])[CH3:4]