huagongshe.com
HRID228106

反应详情

EQUATION

反应方程式

HRID 228106 的结构方程式

REACTANTS

反应物

4
结构：c1ccncc1
HCID1049

Pyridine

C5H5N

结构：O=S(=O)(Cl)Cc1ccccc1
HCID74740

Benzenemethanesulfonyl chloride

C7H7ClO2S

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)N1Cc2ccccc2C[C@H]1C(=O)N[C@H](Cc1ccc(Cl)cc1)C(=O)N1CCN(c2ccccc2N)CC1
HCID58714321

未命名化合物

PRODUCTS

生成物

2
结构：O=C(N[C@H](Cc1ccc(Cl)cc1)C(=O)N1CCN(c2ccccc2NS(=O)(=O)Cc2ccccc2)CC1)[C@@H]1Cc2ccccc2CN1
HCID10146483

未命名化合物

收率 95.9%
结构：CC(C)(C)OC(=O)N1Cc2ccccc2C[C@H]1C(=O)N[C@H](Cc1ccc(Cl)cc1)C(=O)N1CCN(c2ccccc2NS(=O)(=O)Cc2ccccc2)CC1
HCID69079094

未命名化合物

PROCEDURE

实验过程

tert-Butyl 3-(N-{(1R)-1-[(4-chlorophenyl)methyl]-2-oxo-2-[4-(2-{[benzylsulfonyl]amino}phenyl)piperazinyl]ethyl}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-aminophenyl)piperazinyl]-1-[(4-chlorophenyl)methyl]-2-oxoethyl}carbamoyl)(3S)-1,2,3,4-tetrahydroisoquinoline-2-carboxylate (Preparation IX) (730 mg, 1.2 mmol), pyridine (100 μl, 1.2 mmol) and α-toluenesulfonyl chloride (240 mg, 1.2 mmol) (Aldrich). The crude material was purified by flash chromatography (SiO2 10% EtOAc in CH2Cl2) to afford the desired compound (387 mg). MS (ESI, pos. ion) m/z: 772 (M+H), (ESI, neg. ion) m/z: 770 (M−H). Calc'd for C41H46ClN5O6S: 772.35. Anal. Calcd for C41H46ClN5O6S-0.5 C4H8O2: C, 63.26; H, 6.17; N, 8.58; Cl, 4.34. Found C, 62.98; H, 6.09; N, 8.36.

WORKUP

后处理

  1. customThe crude material was purified by flash chromatography (SiO2 10% EtOAc in CH2Cl2)