반응 #3806

ord-633d84603ffe4743a9aba35936f4eeaa

반응 방정식

O=C(Cl)c1ccccc1SSc1ccccc1C(=O)Cl
2,2'-dithiobisbenzoyl chloride
CC(C)(C)c1ccc(N)cc1
4-tert-butylaniline
CC(C)(C)c1ccc(NC(=O)c2ccccc2SSc2ccccc2C(=O)Nc2ccc(C(C)(C)C)cc2)cc1
title compound
수율 12.1%
CC(C)(C)c1ccc(NC(=O)c2ccccc2SSc2ccccc2C(=O)Nc2ccc(C(C)(C)C)cc2)cc1
2,2'-Dithiobis[N-[4-(1,1-dimethylethyl)phenyl]benzamide]
수율 12.1%

반응 조건

온도
23°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축The mixture was concentrated
  2. 2
    기타the residue triturated with 5% aqueous HCl
  3. 3
    여과the resulting solid was collected by filtration
  4. 4
    세척washed with water
  5. 5
    기타to yield the crude product
  6. 6
    기타The crude material was recrystallized from ethyl ether-ethanol

실험 절차

A solution of 2,2'-dithiobisbenzoyl chloride (1.20 g, 3.50 mmol) in 25 mL of dichloromethane was added to a solution of 4-tert-butylaniline (1.04 g, 6.99 mmol) in 8 mL of pyridine at 23° C. The reaction mixture was stirred for 18 hours at 23° C. under nitrogen atmosphere. The mixture was concentrated, the residue triturated with 5% aqueous HCl, and the resulting solid was collected by filtration and washed with water to yield the crude product. The crude material was recrystallized from ethyl ether-ethanol to yield 0.24 g of the title compound, mp 135°-138° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05734081uspto-grants-1998_03