Water → HCID 9816197、化合物

HRID 586795ノート

反応式

HRID 586795 の反応式
[OH:1][CH:2]([CH3:17])[C:3]([NH:6][C:7](=[O:16])[C:8]1[CH:13]=[CH:12][C:11]([F:14])=[CH:10][C:9]=1[F:15])([CH3:5])[CH3:4].C(N(CC)CC)C.O>CS(C)=O>[O:1]=[C:2]([CH3:17])[C:3]([NH:6][C:7](=[O:16])[C:8]1[CH:13]=[CH:12][C:11]([F:14])=[CH:10][C:9]=1[F:15])([CH3:4])[CH3:5]

参加物

5

反応物 3

HCID 962WaterHCID 8471TriethylamineHCID 9816246HCID 9816246、化合物

生成物 1

HCID 9816197HCID 9816197、化合物収率 82.9%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

To a solution of N-(2-hydroxy-1,1-dimethylpropyl)-2,4-difluorobenzamide obtained in Example 33 (0.30 g, 1.2 mmol) and triethylamine (0.37 g, 3.7 mmol) in DMSO (3 ml) was added pyridine sulfur trioxide complex (0.59 g, 3.7 mmol) portionwise and stirred at room temperature for 3 hours. The reaction mixture was added to a mixture of ice and water and extracted with ethyl acetate. The extract was washed with 1N hydrochloric acid, saturated aqueous NaHCO3 and brine, successively dried over Na2SO4 and concentrated under a reduced pressure. The residue was crystallized from hexane/ethyl acetate to give the title compound (0.24 g; 81%).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with 1N hydrochloric acid, saturated aqueous NaHCO3 and brine
  3. dry with materialsuccessively dried over Na2SO4
  4. concentrationconcentrated under a reduced pressure
  5. customThe residue was crystallized from hexane/ethyl acetate

出典と根拠

ORDレコード
ord-28919325596b47d9b18815170a447f56
出典データセット
uspto-grants-2005_08
特許番号
US06936736B2

反応ノート

読み込み中…