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HRID228098

反应详情

EQUATION

反应方程式

HRID 228098 的结构方程式

REACTANTS

反应物

4
结构：c1ccncc1
HCID1049

Pyridine

C5H5N

结构：CS(=O)(=O)Cl
HCID31297

Methanesulfonyl chloride

CH3ClO2S

结构：CC(C)(C)OC(=O)N1CCN(c2ccccc2NS(C)(=O)=O)CC1
HCID21935212

未命名化合物

结构：CC(C)(C)OC(=O)NCCNc1ccccc1N1CCN(C(=O)[C@@H](Cc2ccc(Cl)cc2)NC(=O)[C@@H]2Cc3ccccc3CN2C(=O)OC(C)(C)C)CC1
HCID69073578

未命名化合物

PRODUCTS

生成物

1
结构：CC(C)(C)OC(=O)NCCN(c1ccccc1N1CCN(C(=O)[C@@H](Cc2ccc(Cl)cc2)NC(=O)[C@@H]2Cc3ccccc3CN2C(=O)OC(C)(C)C)CC1)S(C)(=O)=O
HCID86590296

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：CN(C)c1ccncc1
催化剂HCID14284

N,N-Dimethylpyridin-4-amine

C7H10N2

结构：ClCCCl
溶剂HCID11

1,2-Dichloroethane

C2H4Cl2

PROCEDURE

实验过程

tert-Butyl 3-[N-((1R)-2-{4-[2-({2-[(tert-butoxy)carbonylamino]ethyl}(methylsulfonyl)amino)phenyl]piperazinyl}-1-[(4-chlorophenyl)methyl]-2-oxoethyl)-carbamoyl](3S)-1,2,3,4-tetrahydroisoquinoline-2-carboxylate was prepared according to the procedure for Preparation III using tert-butyl 3-[N-((1R)-2-{4-[2-({2-[(tert-butoxy) carbonylamino]ethyl}amino)phenyl]piperazinyl}-1-[(4-chlorophenyl)methyl]-2-oxoethyl)carbamoyl](3S)-1,2,3,4-tetrahydroisoquinoline-2-carboxylate (Step 1) (370 mg, 0.45 mmol), methanesulfonyl chloride (41 μl, 0.530 mmol), pyridine (40 μl, 0.495 mmol), DMAP (cat.), and ClCH2CH2Cl (15 mL). The crude material was purified by flash chromatography, (SiO2, 1:1 hexane:EtOAc) to afford the desired material (155 mg). MS (ESI, pos. ion) m/z: 839 (M+H), (ESI, neg. ion) m/z: 837 (M−H). Calc'd for C42H55ClN6O8S: 839.44.

WORKUP

后处理

  1. customThe crude material was purified by flash chromatography, (SiO2, 1:1 hexane:EtOAc)