反応 #8698

ord-50ab374672784712afdda58eb7ef9ef4

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他Bulk of the solvent was evaporated before it
  2. 2
    workup.ADDITIONwas diluted with diethyl ether (50 ml)
  3. 3
    その他The precipitate that formed
  4. 4
    その他was collected
  5. 5
    洗浄washed with diethyl ether (100 ml)
  6. 6
    その他dried

実験手順

A solution of 4,6-dichloro-5-(2-methoxyphenoxy)-2-(4-pyridyl)-pyrimidine (2 g) and 2-phenyl-ethanesulfonic acid amide potassium salt (2.82 g, Referential Example 1e) in DMF (50 ml) was stirred at rt for 16 h. Bulk of the solvent was evaporated before it was diluted with diethyl ether (50 ml). The mixture was acidified with 10% aq. citric acid. The precipitate that formed was collected, washed with diethyl ether (100 ml) and dried to give 2-phenyl-ethanesulfonic acid [6-chloro-5-(2-methoxy-phenoxy)-2-pyridin-4-yl-pyrimidin-4-yl]-amide (2.23 g) as a beige powder. LC-MS: tR=4.93 min, [M+1]+=497.22, [M−1]−=494.96.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07091201B2uspto-grants-2006_08