(Dimethyl-1,3-thiazol-5-yl)methanol → 2,4-Dimethyl-1,3-thiazole-5-carbaldehyde

HRID 587067ノート

反応式

HRID 587067 の反応式
[CH3:1][C:2]1[S:3][C:4]([CH2:8][OH:9])=[C:5]([CH3:7])[N:6]=1>C1COCC1.[O-2].[O-2].[Mn+4]>[CH3:1][C:2]1[S:3][C:4]([CH:8]=[O:9])=[C:5]([CH3:7])[N:6]=1

参加物

4

反応物 1

HCID 2776250(Dimethyl-1,3-thiazol-5-yl)methanol

生成物 1

HCID 27762492,4-Dimethyl-1,3-thiazole-5-carbaldehyde収率 32.5%

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

In THF (20 ml) was dissolved (2,4-dimethyl-1,3-thiazol-5-yl)methanol (1.0 g). To the solution was added active manganese dioxide (6.0 g), and the mixture was stirred at room temperature for 3 hours. To the mixture was added active manganese dioxide (3.0 g), and the mixture was stirred at room temperature for 1 hour. The mixture was filtered with Celite and washed with methanol. The solvent was removed under reduced pressure, and the resulting residue was purified with silica gel column chromatography (hexane/ethyl acetate/methanol=10/10/1) to give 2,4-dimethyl-1,3-thiazole-5-carbaldehyde (0.32 g).

後処理

  1. stirringthe mixture was stirred at room temperature for 1 hour
  2. filtrationThe mixture was filtered with Celite
  3. washwashed with methanol
  4. customThe solvent was removed under reduced pressure
  5. customthe resulting residue was purified with silica gel column chromatography (hexane/ethyl acetate/methanol=10/10/1)

出典と根拠

ORDレコード
ord-bae70c39265a4155985234f3c929fffd
出典データセット
uspto-grants-2005_08
特許番号
US06936602B1

反応ノート

読み込み中…