Reaktion #46960

ord-c44cdadaf62e49d08894edeb08909e47

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeA 500 ml reactor equipped with mechanical stirrer
  2. 2
    Sonstigethe temperature below 30° C.
  3. 3
    workup.ADDITIONduring the addition the solid
  4. 4
    workup.DISSOLUTIONgradually solubilized until complete dissolution
  5. 5
    Filtrationafter approx. 1 hour the precipitated white solid was filtered
  6. 6
    Waschenwashed with 70 ml of water
  7. 7
    Sonstigedried

Vorschrift

A 500 ml reactor equipped with mechanical stirrer, thermometer and condenser was loaded with 200 ml of water, 30 g of 2-acetylamino-4,5,6,7-tetrahydro-benzothiazole-6-carboxylic acid ethyl ester [(II), R1=ethyl, R=—NH—CO—CH3] and 52.2 g of 30% sodium hydroxide, keeping the temperature below 30° C.; during the addition the solid gradually solubilized until complete dissolution. After 2 hours, glacial acetic acid was dropwise added to pH=4.5-5.5; after approx. 1 hour the precipitated white solid was filtered, washed with 70 ml of water and dried to obtain 24.8 g of 2-acetylamino-4,5,6,7-tetrahydro-benzothiazole-6-carboxylic acid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07741490B2uspto-grants-2010_06