Methyl iodide → 4-Bromo-2-isopropyl-7-methoxymethyl-2H-phthalazin-1-one

HRID 1765356ノート

反応式

HRID 1765356 の反応式
[Br:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([CH2:12][OH:13])=[CH:9][CH:10]=2)[C:5](=[O:14])[N:4]([CH:15]([CH3:17])[CH3:16])[N:3]=1.[H-].[Na+].[CH3:20]I>C1COCC1>[Br:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([CH2:12][O:13][CH3:20])=[CH:9][CH:10]=2)[C:5](=[O:14])[N:4]([CH:15]([CH3:17])[CH3:16])[N:3]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 21106569HCID 21106569、化合物

生成物 1

HCID 211065634-Bromo-2-isopropyl-7-methoxymethyl-2H-phthalazin-1-one収率 69.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

4-Bromo-7-hydroxymethyl-2-isopropyl-2H-phthalazin-1-one (0.11 g, 0.37 mmol) was dissolved in THF (2 ml). To this was added NaH (60%, 0.019 g, 0.44 mmol) as a THF suspension (2 ml). To this was added methyl iodide (0.063 g, 0.48 mmol) and the reaction mixture was stirred for 20 hours. The reaction mixture was concentrated under vacuum and the residue was purified by flash column chromatography (elution: 80% heptane, 20% ethyl acetate) to give the title compound (0.08 g, 69% yield) as a white solid.

後処理

  1. concentrationThe reaction mixture was concentrated under vacuum
  2. customthe residue was purified by flash column chromatography (elution: 80% heptane, 20% ethyl acetate)

出典と根拠

ORDレコード
ord-81299beceee74fbb98c3b11d18ee5e41
出典データセット
uspto-grants-2007_06
特許番号
US07226923B2

反応ノート

読み込み中…