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HRID1396926

反应详情

EQUATION

反应方程式

HRID 1396926 的结构方程式

REACTANTS

反应物

1
结构：C[C@H]1CN(C)CCN1c1nccc(NC(=O)[C@@H]2CCN(C(=O)OCc3ccccc3)N2C(=O)[C@H](CC2CCCC2)CN(C=O)OCc2ccccc2)n1
HCID86706365

未命名化合物

PRODUCTS

生成物

1
结构：C[C@H]1CN(C)CCN1c1nccc(NC(=O)[C@@H]2CCNN2C(=O)[C@H](CC2CCCC2)CN(O)C=O)n1
HCID66546324

未命名化合物

收率 75.1%

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

A mixture of phenylmethyl (3S)-2-[(2R)-3-cyclopentyl-2-({formyl[(phenylmethyl)oxy]amino}methyl)propanoyl]-3-[({2-[(2S)-2,4-dimethyl-1-piperazinyl]-4-pyrimidinyl}amino) carbonyl]-1-pyrazolidinecarboxylate (236 mg, 0.325 mmol) and Pearlman's catalyst (45.6 mg, 0.065 mmol) in methanol (1.81 ml) was degassed and placed under 1 atm of H2 at ambient temperature. After 2 hrs, the reaction mixture was filtered and concentrated to give a residue which was purified by RP-HPLC to give (3S)-2-((2R)-3-cyclopentyl-2-{[formyl(hydroxy)amino]methyl}propanoyl)-N-{2-[(2S)-2,4-dimethyl-1-piperazinyl]-4-pyrimidinyl}-3-pyrazolidine carboxamide (125 mg, 0.244 mmol, 75% yield). MS (ES+) m/z 503.1 (MH+).

WORKUP

后处理

  1. customwas degassed
  2. customplaced under 1 atm of H2 at ambient temperature
  3. filtrationthe reaction mixture was filtered
  4. concentrationconcentrated
  5. customto give a residue which
  6. customwas purified by RP-HPLC