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HRID1242730

反应详情

EQUATION

反应方程式

HRID 1242730 的结构方程式

REACTANTS

反应物

3
结构：CS(=O)(=O)Cl
HCID31297

Methanesulfonyl chloride

CH3ClO2S

结构：CC(C)(C)c1cccc(C(C)(C)C)n1
HCID68510

2,6-Di-tert-butylpyridine

C13H21N

结构：Nc1ccccc1N1CCN(C(=O)[C@@H](Cc2ccc(Cl)cc2)NC(=O)[C@H]2Cc3ccccc3CN2C(=O)OCC2c3ccccc3-c3ccccc32)CC1
HCID58714327

未命名化合物

PRODUCTS

生成物

1
结构：CS(=O)(=O)Nc1ccccc1N1CCN(C(=O)[C@@H](Cc2ccc(Cl)cc2)NC(=O)[C@H]2Cc3ccccc3CN2C(=O)OCC2c3ccccc3-c3ccccc32)CC1
HCID58714322

未命名化合物

收率 86.3%

PROCEDURE

实验过程

Fluoren-9-ylmethyl (3R)-3-{N-[(1R)-1-[(4-chlorophenyl)methyl]-2-(4-{2-[(methylsulfonyl)amino] phenylpiperazinyl)-2-oxoethyl]carbamoyl}-1,2,3,4-tetrahydroisoquinoline-2-carboxylate was prepared from fluoren-9-ylmethyl (3R)-3-(N-{(1R)-2-[4-(2-aminophenyl)piperazinyl]-1-[(4-chlorophenyl)methyl]-2-oxoethyl}carbamoyl)-1,2,3,4-tetrahydroisoquinoline-2-carboxylate (250 mg, 0.34 mmol) according to the procedure for Preparation III using methanesulfonyl chloride (30 μl, 0.39 mmol) and 2,6-di-tert-butyl-pyridine (80 μl, 0.36 mmol) (Aldrich). The crude product was concentrated in vacuo and purified by flash chromatography (SiO2, 15% EtOAc in CH2Cl2), to afford the desired compound (240 mg). MS (ESI, pos. ion) m/z: 818 (M+H), (ESI, neg. ion) m/z: 816 (M−H). Calc'd for C45H44ClN5O6S: 817.27.

WORKUP

后处理

  1. concentrationThe crude product was concentrated in vacuo
  2. custompurified by flash chromatography (SiO2, 15% EtOAc in CH2Cl2)