Reaktion #322819

ord-4128f83a82374103b87f503118da9ba2

Reaktionsgleichung

COc1ccc(N)c(S)c1
2-amino-5-methoxythiophenol
COC(=O)C(Br)CCBr
methyl 2,4-dibromobutyrate
COc1ccc2c(c1)SC(CCBr)C(=O)N2
2-(2-bromoethyl)-7-methoxy-2H-1,4-benzothiazin-3(4H)-one
Ausbeute 65.3%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationthe resulting crystals were collected by filtration
  2. 2
    Waschenwashed with water
  3. 3
    SonstigeRecrystallization from methanol

Vorschrift

A solution of 3.10 g of 2-amino-5-methoxythiophenol and 5.20 g of methyl 2,4-dibromobutyrate in 30 ml of dimethylformamide was stirred at room temperature for 2 hours. The mixture was poured into ice-water and the resulting crystals were collected by filtration and washed with water. Recrystallization from methanol gave 3.94 g (65.2%) of 2-(2-bromoethyl)-7-methoxy-2H-1,4-benzothiazin-3(4H)-one as prisms, m.p. 142°-143° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04640916uspto-grants-1987_02