m-Chloroperbenzoic acid → 3-bromo-2-methylthieno[2,3-c]pyridine-N-Oxide

HRID 1668967ノート

反応式

HRID 1668967 の反応式
[Br:1][C:2]1[C:10]2[C:5](=[CH:6][N:7]=[CH:8][CH:9]=2)[S:4][C:3]=1[CH3:11].ClC1C=CC=C(C(OO)=[O:20])C=1>C(Cl)Cl.[OH-].[Na+]>[Br:1][C:2]1[C:10]2[C:5](=[CH:6][N+:7]([O-:20])=[CH:8][CH:9]=2)[S:4][C:3]=1[CH3:11]

参加物

5

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 584664443-Bromo-2-methylthieno[2,3-c]pyridine

生成物 1

HCID 673397463-bromo-2-methylthieno[2,3-c]pyridine-N-Oxide

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回HCID 14798Sodium Hydroxide溶媒

実験手順

3-Bromo-2-methylthieno[2,3-c]pyridine (0.500 g, 2.19 mmol) was dissolved in DCM (10 ml) and cooled down to 0° C. m-Chloroperbenzoic acid (0.737 g, 3.29 mmol) was added to the reaction portionwise while stirring. After 4 hours, the reaction wad diluted with 1N NaOH (10 ml) and DCM (10 ml). The layers were separated and the organic layer was washed (2×) with an aqueous saturated solution of sodium bicarbonate, then with water and then brine. The organic layer was then dried with sodium sulfate, reduced in vacuo and dried to give the title compound as a yellow solid. MS (M+H)+ 245

後処理

  1. additionwas added to the reaction portionwise
  2. customThe layers were separated
  3. washthe organic layer was washed (2×) with an aqueous saturated solution of sodium bicarbonate
  4. dry with materialThe organic layer was then dried with sodium sulfate
  5. customdried

出典と根拠

ORDレコード
ord-b7a585f472134f77baf0293917fbb97e
出典データセット
uspto-grants-2011_08
特許番号
US07989461B2

反応ノート

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