m-Chloroperbenzoic acid → N-methyl-4-(2-(methylsulfinyl)benzo[d]oxazol-6-yloxy)picolinamide

HRID 2370491

反応式

HRID 2370491 の反応式
[CH3:1][S:2][C:3]1[O:4][C:5]2[CH:11]=[C:10]([O:12][C:13]3[CH:18]=[CH:17][N:16]=[C:15]([C:19]([NH:21][CH3:22])=[O:20])[CH:14]=3)[CH:9]=[CH:8][C:6]=2[N:7]=1.ClC1C=C(C=CC=1)C(OO)=[O:28]>C(Cl)Cl>[CH3:1][S:2]([C:3]1[O:4][C:5]2[CH:11]=[C:10]([O:12][C:13]3[CH:18]=[CH:17][N:16]=[C:15]([C:19]([NH:21][CH3:22])=[O:20])[CH:14]=3)[CH:9]=[CH:8][C:6]=2[N:7]=1)=[O:28]

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 577256324-(2-(methylthio)benzo[d]oxazol-6-yloxy)-N-methylpyridine-2-carboxamide

生成物 1

HCID 57725414N-methyl-4-(2-(methylsulfinyl)benzo[d]oxazol-6-yloxy)picolinamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of the 4-(2-(methylthio)benzo[d]oxazol-6-yloxy)-N-methylpyridine-2-carboxamide (1.26 g, 4.0 mmol, 1.0 eq) in 40 mL of methylene chloride was added 3-chloroperoxybenzoic acid (70%, 989 mg, 4.4 mmol, 1.1 eq). The reaction mixture was stirred at room temperature for 5 hours and then was diluted with 200 mL of methylene chloride. The resulting mixture was washed with aqueous sodium bicarbonate and brine then dried over MgSO4, filtered, and evaporated under reduced pressure to give crude product, which was used to next step without further purification. MH+=332.

後処理

  1. washThe resulting mixture was washed with aqueous sodium bicarbonate and brine
  2. dry with materialthen dried over MgSO4
  3. filtrationfiltered
  4. customevaporated under reduced pressure
  5. customto give crude product, which
  6. customwas used to next step without further purification

出典と根拠

ORDレコード
ord-2f95c9273f754826ab92d205e93c6594
出典データセット
uspto-grants-2014_04
特許番号
US08710048B2

関連ノート

読み込み中…