反応 #334651

ord-cc3cf87295054356b17909d3b9a248d0

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮the mixture is concentrated in vacuo
  2. 2
    抽出the insoluble constituents are extracted with methylene chloride
  3. 3
    抽出extracted with methylene chloride
  4. 4
    乾燥The methylene chloride solution is dried over sodium sulfate
  5. 5
    濃縮concentrated

実験手順

A mixture of 14.2 g of N-(3-chloropyridazine-6-sulfonyl)phenylcarbamate and 6.3 g of 2-amino-4-methoxy-6-methyl-1,3,5-triazine are refluxed for 1 hour in 120 ml of absolute dioxan. When the reaction is complete, the mixture is concentrated in vacuo and the residue is taken up in a saturated aqueous solution of sodium bicarbonate and the insoluble constituents are extracted with methylene chloride. The aqueous phase is acidified with dilute hydrochloric acid and extracted with methylene chloride. The methylene chloride solution is dried over sodium sulfate and concentrated, affording 7 g of the compound of the above formula with a melting point of 135° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04707551uspto-grants-1987_11