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HRID489666

反应详情

EQUATION

反应方程式

HRID 489666 的结构方程式

REACTANTS

反应物

5
结构：ClCCCl
HCID11

1,2-Dichloroethane

C2H4Cl2

结构：O=C(O)C(F)(F)F
HCID6422

未命名化合物

结构：On1nnc2ccccc21
HCID75771

1-Hydroxybenzotriazole

C6H5N3O

结构：CC(C)(C)OC(=O)N1CCC1C(=O)O
HCID3623886

1-(tert-Butoxycarbonyl)azetidine-2-carboxylic acid

C9H15NO4

结构：CC(C)(C)OC(=O)N[C@H](Cc1ccc(Cl)cc1)C(=O)N1CCC(c2ccccc2N(CC2CC2)S(C)(=O)=O)CC1
HCID23587431

未命名化合物

PRODUCTS

生成物

1
结构：CC(C)(C)OC(=O)N1CC(C(=O)N[C@H](Cc2ccc(Cl)cc2)C(=O)N2CCC(c3ccccc3N(CC3CC3)S(C)(=O)=O)CC2)C1
HCID23587442

未命名化合物

收率 71.3%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：ClCCl
溶剂HCID6344

Dichloromethane

CH2Cl2

结构：C1CCOC1
溶剂HCID8028

Tetrahydrofuran

C4H8O

PROCEDURE

实验过程

The title compound was prepared according to the procedure described in Example 11 (Step c) using N-[(1R)-1-[(4-chlorophenyl)methyl]-2-(4-{2-[(cyclopropylmethyl)-(methylsulfonyl)amino]phenyl}-piperidyl)-2-oxoethyl](tert-butoxy)carboxamide (Example 11 Step b) (450 mg, 0.76 mmol) and 50% TFA in CH2Cl2 (6 mL) followed by EDC (Aldrich) (259 mg, 1.35 mmol), HOBT (Aldrich) (270 mg, 2.0 mmol) and N-Boc-azetidine-4-carboxylic acid (PepTech Corporation) (220 mg, 1.1 mmol) in THF (20 mL). Purification by silica gel chromatography (10:25:65 MeOH:EtOAc:hexane) provided the title compound as a white foam (365 mg). MS (ESI, pos. ion) m/z: 673 (M+1); (ESI, neg. ion) m/z: 671 (M−1). Calc'd for C34H45ClN4O6S: 673.26.

WORKUP

后处理

  1. customThe title compound was prepared
  2. customPurification by silica gel chromatography (10:25:65 MeOH:EtOAc:hexane)