反应 #2358563

ord-a893ec201ae04fd2bfd4ac66f530c158

反应方程式

O=C1c2ccc(S(=O)(=O)Cl)cc2C(=O)c2cc(S(=O)(=O)Cl)ccc21
Anthraquinone-2,7-disulfonylchloride
CC(C)(C)C1CCC(N)CC1
4-tert-butylcyclohexanamine
CCN(CC)CC
triethyl amine
CC(C)(C)C1CCC(NS(=O)(=O)c2ccc3c(c2)C(=O)c2cc(S(=O)(=O)NC4CCC(C(C)(C)C)CC4)ccc2C3=O)CC1
product ( 1-36 )
CC(C)(C)C1CCC(NS(=O)(=O)c2ccc3c(c2)C(=O)c2cc(S(=O)(=O)NC4CCC(C(C)(C)C)CC4)ccc2C3=O)CC1
N2,N7-bis(4-tert-butylcyclohexyl)-9,10-dioxo-9,10-dihydroanthracene-2,7-disulfonamide

溶剂

反应条件

温度
-50°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他Solvent was evaporated
  2. 2
    workup.ADDITIONthe residue was treated with MeOH
  3. 3
    过滤filtered off
  4. 4
    其他dried

实验过程

Anthraquinone-2,7-disulfonylchloride (10 g, 24.7 mmol)) was dissolved in 200 mL DCM. The solution was cooled to −50° C. To this solution was added 4-tert-butylcyclohexanamine (8.43 g, 54 mmol), followed by triethyl amine (8.6 ml, 61:7 mmol). The reaction mixture was stirred at room temperature for 4 hrs. Solvent was evaporated and the residue was treated with MeOH, filtered off, and dried to obtain 15 g (95%) of the product (1-36) as yellow powder.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09120754B2uspto-grants-2015_09