huagongshe.com
HRID1366685

反应详情

EQUATION

反应方程式

HRID 1366685 的结构方程式

REACTANTS

反应物

1
结构：Cc1nc(NNC(=O)[C@H](CC2CCCC2)CN(C=O)OCc2ccccc2)c(F)c(N2CCOC[C@@H]2C)n1
HCID86637030

未命名化合物

PRODUCTS

生成物

1
结构：Cc1nc(NNC(=O)[C@H](CC2CCCC2)CN(O)C=O)c(F)c(N2CCOC[C@@H]2C)n1
HCID58000539

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：[OH-].[OH-].[Pd+2]
催化剂HCID9942167

Palladium hydroxide

H2O2Pd

结构：CO
溶剂HCID887

Methanol

CH4O

PROCEDURE

实验过程

To a solution of [(2R)-2-(cyclopentylmethyl)-3-(2-{5-fluoro-2-methyl-6-[(3S)-3-methyl-4-morpholinyl]-4-pyrimidinyl}hydrazino)-3-oxopropyl][(phenylmethyl)oxy]formamide (309.1 mg, 0.563 mmol) in methanol (6 mL) was added 20% Pd(OH)2/C (50% water, 62 mg). The suspension was hydrogenated for 1 h and then filtered through a PTFE membrane. The resulting solution was concentrated in vacuo and purified by Gilson RPLC to give [(2R)-2-(cyclopentylmethyl)-3-(2-{5-fluoro-2-methyl-6-[(3S)-3-methyl-4-morpholinyl]-4-pyrimidinyl}hydrazino)-3-oxopropyl]hydroxyformamide (94.0 mg, 36%) as a white solid following crystallization from EtOAc-Et2O. LCMS: (M+H)+: 459.1.

WORKUP

后处理

  1. filtrationfiltered through a PTFE membrane
  2. concentrationThe resulting solution was concentrated in vacuo
  3. custompurified by Gilson RPLC
  4. customto give
  5. custom[(2R)-2-(cyclopentylmethyl)-3-(2-{5-fluoro-2-methyl-6-[(3S)-3-methyl-4-morpholinyl]-4-pyrimidinyl}hydrazino)-3-oxopropyl]hydroxyformamide (94.0 mg, 36%) as a white solid following crystallization from EtOAc-Et2O