반응 #2261635

ord-f52ff8428ecb45a2b21b1eb3f6ef4775

시약

없음

용매

반응 조건

온도
100°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The mixture was evaporated
  2. 2
    기타co-evaporated 3×50 ml of water, and crystallized with water/acetone

실험 절차

Methyl 4-azido-2-sulfo-butyrate (1.00 g, 4.08 mmol) in the mixture of HCl (50 ml, 1.0 M) and HAC (5 ml) was heated at 100° C. for 8 hrs. The mixture was evaporated and co-evaporated 3×50 ml of water, and crystallized with water/acetone to afford 1.0 g (99%) of the title compound. 1H NMR (DMF-d7): 3.60 (m, 2H), 3.52 (m, 1H), 2.24 (m, 2H). 13C NMR 170.96, 63.04, 50.66, 29.12. ESI MS m/z−207.7 (MW−H); HRMS m/z−(C4H7N3O5S—H) calcd 208.0028. found 208.0021.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09061995B2uspto-grants-2015_06