1-(6-Chloro-3-methoxy-pyridazin-4-yl)-propan-1-ol → 1-(6-Chloro-3-methoxy-pyridazin-4-yl)-propan-1-one

HRID 1786694ノート

反応式

HRID 1786694 の反応式
[Cl:1][C:2]1[N:7]=[N:6][C:5]([O:8][CH3:9])=[C:4]([CH:10]([OH:13])[CH2:11][CH3:12])[CH:3]=1>O1CCCC1.[O-2].[O-2].[Mn+4]>[Cl:1][C:2]1[N:7]=[N:6][C:5]([O:8][CH3:9])=[C:4]([C:10](=[O:13])[CH2:11][CH3:12])[CH:3]=1

参加物

4

反応物 1

HCID 102622801-(6-Chloro-3-methoxy-pyridazin-4-yl)-propan-1-ol

生成物 1

HCID 230924891-(6-Chloro-3-methoxy-pyridazin-4-yl)-propan-1-one

試薬・触媒・溶媒 2

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

実験手順

12.25 g 1-(6-Chloro-3-methoxy-pyridazin-4-yl)-propan-1-ol is dissolved in 410 ml tetrahydrofuran and 105 g of manganese dioxide is added. The reaction is stirred for 24 h at RT. Solids are removed by filtration, and the solution is treated with a further 105 g of manganese dioxide for 16 h at RT. Solids are removed by filtration, and the solvent is removed under reduced pressure. The product is purified by silica gel chromatography, eluting with a gradient of ethyl acetate in heptane. Yield 3.25 g. LC-MS (ES+) 201 (M+H)+.

後処理

  1. customSolids are removed by filtration
  2. additionthe solution is treated with a further 105 g of manganese dioxide for 16 h at RT
  3. customSolids are removed by filtration
  4. customthe solvent is removed under reduced pressure
  5. customThe product is purified by silica gel chromatography
  6. washeluting with a gradient of ethyl acetate in heptane

出典と根拠

ORDレコード
ord-695cb214ce6b4accb0e739d2448d5410
出典データセット
uspto-grants-2009_03
特許番号
US07507734B2

反応ノート

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