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HRID489652

反应详情

EQUATION

反应方程式

HRID 489652 的结构方程式

REACTANTS

反应物

2
结构：O=C(O)C(F)(F)F
HCID6422

未命名化合物

结构：CC(C)(C)OC(=O)N[C@H]1CC[C@@H](C(=O)N[C@H](Cc2ccc(Cl)cc2)C(=O)N2CCC(c3ccccc3NS(C)(=O)=O)CC2)C1
HCID69151551

未命名化合物

PRODUCTS

生成物

1
结构：CS(=O)(=O)Nc1ccccc1C1CCN(C(=O)[C@@H](Cc2ccc(Cl)cc2)NC(=O)[C@@H]2CC[C@H](N)C2)CC1
HCID10119929

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：ClCCl
溶剂HCID6344

Dichloromethane

CH2Cl2

PROCEDURE

实验过程

To a 50 mL round-bottomed flask was added N-[(1R)-1-[(4-chlorophenyl)methyl]-2-(4-{2-[(methylsulfonyl)-amino]phenyl}-piperidyl)-2-oxoethyl]{(3S, 1R)-3-[(tert-butoxy)carbonylamino]-cyclopentyl)-carboxamide (Step a) (323 mg, 0.5 mmol) followed by a 50% soln of TFA in CH2Cl2 (20 mL). After stirring for 2 h, the solvent was removed in vacuo. Purification by preparative HPLC [Phenomenex; 5 μm 250×21.2 mm, 5% to 95% CH3CN (0.1% TFA) in H2O (0.1% TFA) over 30 min, then 100% CH3CN (0.1% TFA) for 2 min]provided the title compound (TFA salt) as a white foam (145 mg). MS (ESI, pos. ion) m/z: 547 (M+1); (ESI, neg. ion) 545 (M−1). Calc'd for C27H35ClN4O4S: 546.21. Anal. Calcd for C27H35ClN4O4S.1.2C2HF3O2: C, 51.63; H, 5.49; N, 8.19. Found: C, 51.69; H, 5.49; N, 8.14.

WORKUP

后处理

  1. customthe solvent was removed in vacuo
  2. customPurification by preparative HPLC [Phenomenex
  3. wait5 μm 250×21.2 mm, 5% to 95% CH3CN (0.1% TFA) in H2O (0.1% TFA) over 30 min