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

HRID 1765356노트

반응식

HRID 1765356 반응식
[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

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 21106569HCID 21106569, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-81299beceee74fbb98c3b11d18ee5e41
출처 데이터셋
uspto-grants-2007_06
특허 번호
US07226923B2

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