Reaktion #605972

ord-ddb76c954bc84961aec8538077e32af3

Reaktionsgleichung

O=S(=O)(O)O
sulfuric acid
[Br-].[Na+]
sodium bromide
[Na+].[O-][Br+2]([O-])[O-]
sodium bromate
COC(=O)c1sc2cnc(SC)nc2c1-c1cccc(OC)n1
methyl 7-(6-methoxypyridin-2-yl)-2-(methylsulfanyl)thieno[3,2-d]pyrimidine-6-carboxylate
COC(=O)c1sc2cnc(S(C)=O)nc2c1-c1cccc(OC)n1
methyl 7-(6-methoxypyridin-2-yl)-2-(methylsulfinyl)thieno[3,2-d]pyrimidine-6-carboxylate

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeprepared by analogy to the method
  2. 2
    Filtrationthe yellow suspension is filtered through a number 4 sintered glass
  3. 3
    Filtrationfilter
  4. 4
    SonstigeThe yellow solid is dried under vacuum so as

Vorschrift

24 mg of sodium bromide and 18 mg of sodium bromate are added, with stirring, to a suspension of 55 mg of methyl 7-(6-methoxypyridin-2-yl)-2-(methylsulfanyl)thieno[3,2-d]pyrimidine-6-carboxylate, prepared by analogy to the method described in example 5, (at 50%) in 2 ml of water, and then 6.5 μl of concentrated sulfuric acid are slowly added. The yellow suspension rapidly turns orange. After 2 h 30 minutes of stirring at ambient temperature, the yellow suspension is filtered through a number 4 sintered glass filter. The yellow solid is dried under vacuum so as to obtain 28 mg of methyl 7-(6-methoxypyridin-2-yl)-2-(methylsulfinyl)thieno[3,2-d]pyrimidine-6-carboxylate.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09115140B2uspto-grants-2015_08