반응 #86544

ord-92f53ceabd6d4381b252a49e4df22896

반응 방정식

Nc1nccs1
1,3-thiazol-2-amine
COC(=O)CC(=O)C(C)Br
methyl 4-bromo-3-oxopentanoate
CC(Br)c1cc(=O)n2ccsc2n1
7-(1-bromoethyl)-5H-[1,3]thiazolo[3,2-a]pyrimidin-5-one

반응 조건

온도
110°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도After cooling
  2. 2
    여과The mixture was filtered
  3. 3
    기타the collected precipitate was air-dried
  4. 4
    기타to give crude product which

실험 절차

A mixture of polyphosphoric acid (73.8 g, 677 mmol), 1,3-thiazol-2-amine (12.3 g, 123 mmol), and methyl 4-bromo-3-oxopentanoate (34.8 g, 166 mmol) was stirred at 110° C. overnight. After cooling, an ice-cold 10% aq. NaOH solution was slowly added to adjust the pH to 7. The mixture was filtered, and the collected precipitate was air-dried to give crude product which was directly used in next step. LCMS calculated for C8H8BrN2OS (M+H)+: m/z=259.0. Found: 259.0.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09434746B2uspto-grants-2016_09