반응 #620677

ord-1245c93b046441188adfc0390fd784f8

반응 방정식

O=c1c2ccccc2sc2ccc(CBr)cc12
2-bromomethylthioxanthone
OCCN(CCO)CCO
triethanol amine
O=c1c2ccccc2sc2ccc(C[N+](CCO)(CCO)CCO)cc12.[Br-]
white solids
O=c1c2ccccc2sc2ccc(C[N+](CCO)(CCO)CCO)cc12.[Br-]
N-(9-oxo-9H-thioxanthene-2-yl)methyl-N,N,N-tris(2-hydroxyethyl)ammonium bromide

반응 조건

온도
25°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONafter the addition)
  2. 2
    기타the organic solvent was evaporated under reduced pressure

실험 절차

The intermediate (C122-2-2) (2-bromomethylthioxanthone) (1.0 part) was dissolved in dichloromethane (85 g), and triethanol amine [product of Wako Pure Chemical industries, Ltd.] (0.5 parts) was added dropwise to this solution (an exotherm was observed after the addition). The resulting mixture was stirred at room temperature (about 25° C.) for one hour, and the organic solvent was evaporated under reduced pressure. As a result, 2.2 g of white solids were obtained. The white solids were recrystallized in a tetrahydrofuran/dichloromethane mixed solution, and 1.0 part of an intermediate (C122-2-3) was obtained (as brown solids).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08853290B2uspto-grants-2014_10