반응 #52577

ord-eb8d8b4b51e54713ba1babd8bd6e5d5f

반응 방정식

CC(Br)C(=O)Br
2-Bromopropionyl bromide
NCCS(=O)(=O)O
taurine
[Na+].[OH-]
NaOH
CC(Br)C(=O)NCCS(=O)(=O)[O-].[Na+]
Sodium 2-(2-bromopropionylamino)-ethanesulfonate

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas then added to the solution drop wise at 0° C. over 30 minutes
  2. 2
    workup.ADDITIONDuring the addition
  3. 3
    기타a large amount of solid was produced
  4. 4
    workup.ADDITIONto thoroughly mix the compounds until no more exotherm
  5. 5
    여과The solid was filtered
  6. 6
    세척washed with a small amount of absolute ethanol
  7. 7
    건조ethyl ether and then dried in vacuo
  8. 8
    기타recrystallized from methanol

실험 절차

25.6 g of taurine (204 mmol) and 16.38 g of NaOH (409 mmol) were dissolved in 20 ml of deionized water. 2-Bromopropionyl bromide (44 g, 21.36 ml, 204 mmol) dissolved in 50 ml of dichloromethane was then added to the solution drop wise at 0° C. over 30 minutes. During the addition, a large amount of solid was produced. The reaction flask was manually agitated to thoroughly mix the compounds until no more exotherm was observed with additional agitation. The reaction mixture was then allowed to sit for 1 hour. The solid was filtered and washed with a small amount of absolute ethanol and then ethyl ether and then dried in vacuo. The compound can be used in this state or recrystallized from methanol.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06855840B2uspto-grants-2005_02