N-bromobutanimide → 7-Bromo-4-methoxy-2-methylsulfanylbenzooxazole

HRID 2186445

反応式

HRID 2186445 の反応式
[Br:1]N1C(=O)CCC1=O.[CH3:9][O:10][C:11]1[C:16]2[N:17]=[C:18]([S:20][CH3:21])[O:19][C:15]=2[CH:14]=[CH:13][CH:12]=1>C(#N)C>[Br:1][C:14]1[C:15]2[O:19][C:18]([S:20][CH3:21])=[N:17][C:16]=2[C:11]([O:10][CH3:9])=[CH:12][CH:13]=1

参加物

4

反応物 2

HCID 67184N-bromobutanimideHCID 224566644-Methoxy-2-(methylthio)benzo[d]oxazole

生成物 1

HCID 224566517-Bromo-4-methoxy-2-methylsulfanylbenzooxazole収率 33.8%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

N-Bromosuccinimide (2.4 g) was added to a solution of 4-methoxy-2-methylsulfanylbenzooxazole (2.63 g) in acetonitrile (80 ml) and the mixture stirred for 18 hours. It was then partitioned between dichloromethane (200 ml) and water (200 ml). The organics were washed with water (200 ml), dried over magnesium sulphate, filtered and the solvent removed in vacuo. Purification by column chromatography on silica eluting with 10% ethyl acetate in heptane afforded the title compound as a white solid (1.25 g).

後処理

  1. customIt was then partitioned between dichloromethane (200 ml) and water (200 ml)
  2. washThe organics were washed with water (200 ml)
  3. dry with materialdried over magnesium sulphate
  4. filtrationfiltered
  5. customthe solvent removed in vacuo
  6. customPurification by column chromatography on silica eluting with 10% ethyl acetate in heptane

出典と根拠

ORDレコード
ord-721a3691b2b743c5ae80a1caaa429e33
出典データセット
uspto-grants-2002_06
特許番号
US06403791B1

関連ノート

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