huagongshe.com
HRID351381

反应详情

EQUATION

反应方程式

HRID 351381 的结构方程式

REACTANTS

反应物

1
结构：[N-]=[N+]=N[C@@H]1CC[C@H](N2CC[C@H](CC3(c4cccc(C(F)(F)F)c4)OCCO3)C2=O)[C@H](CS(=O)(=O)c2ccccc2)C1
HCID86594365

未命名化合物

PRODUCTS

生成物

1
结构：N[C@@H]1CC[C@H](N2CC[C@H](CC3(c4cccc(C(F)(F)F)c4)OCCO3)C2=O)[C@H](CS(=O)(=O)c2ccccc2)C1
HCID69035635

未命名化合物

收率 80%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：[Pd]
催化剂HCID23938

Palladium

Pd

结构：CO
溶剂HCID887

Methanol

CH4O

PROCEDURE

实验过程

A mixture of 39g-b (222 mg, 375 μmol) and 10% Pd/C (239 mg, 112 μmol) in MeOH (150 mL) was hydrogenated (50 psi) for 2 h. The mixture was filtered through diatomaceous earth (infusorial earth) and the filtrate was evaporated under vacuum to give (R*)-1-((1S*,2R*,4R*)-4-amino-2-(phenylsulfonylmethyl)cyclohexyl)-3-((2-(3-(trifluoromethyl)phenyl)-1,3-dioxolan-2-yl)methyl)pyrrolidin-2-one (39h-b, 169 mg, 80%) as a white solid: 1H NMR (300 MHz, CDCl3) δ 7.87 (d, J=7.3 Hz, 2H), 7.68–7.35 (m, 7H), 4.22 (s, 1H), 4.02–3.60 (m, 5H), 3.50–3.14 (m, 4H), 2.80–2.63 (m, 1H), 2.60–1.60 (m, 12H); 19F NMR (282 MHz, CDCl3) δ −62.8; ESI MS m/z 567 [C28H33F3N2O5S+H]+.

WORKUP

后处理

  1. customfor 2 h
  2. filtrationThe mixture was filtered through diatomaceous earth (infusorial earth)
  3. customthe filtrate was evaporated under vacuum