反应 #998692

ord-a13f3af889d443629a2824fa8c796f36

反应方程式

CN(C)C(=O)Sc1c(Cl)ccc2c1CCN(C(=O)OC(C)(C)C)CC2
3-tert-butoxycarbonyl-7-chloro-6-dimethylcarbamoylthio-2,3,4,5-tetrahydro-1H-benzo[d]azepine
O=C(c1ccccc1)c1ccc(CBr)cc1
4-(bromomethyl)benzophenone
Cl.O=C(c1ccccc1)c1ccc(CSc2c(Cl)ccc3c2CCNCC3)cc1
title compound
Cl.O=C(c1ccccc1)c1ccc(CSc2c(Cl)ccc3c2CCNCC3)cc1
6-(4-Benzoylbenzylthio)-7-chloro-2,3,4,5-tetrahydro-1H-benzo[d]azepine Hydrochloride

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他Purify by preparative reverse phase HPLC (Column: Xterra Prep RP18 19×250 mm; Solvent A: 10 mM aqueous ammonium carbonate, Solvent B: acetonitrile; 30-100% B over 20 minutes; flow rate 25 mL/ruin)

实验过程

Use a method similar to the Example 380 to react 3-tert-butoxycarbonyl-7-chloro-6-dimethylcarbamoylthio-2,3,4,5-tetrahydro-1H-benzo[d]azepine with 4-(bromomethyl)benzophenone. Purify by preparative reverse phase HPLC (Column: Xterra Prep RP18 19×250 mm; Solvent A: 10 mM aqueous ammonium carbonate, Solvent B: acetonitrile; 30-100% B over 20 minutes; flow rate 25 mL/ruin). Use a method similar to the General Procedure 2-2 to give the title compound as a white solid. MS (ES+) m/z: 408 (M+H)+.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08022062B2uspto-grants-2011_09