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

HRID 1783670노트

반응식

HRID 1783670 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% EtOAc) 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% EtOAc)

출처 및 근거

ORD 기록
ord-b4c14feb9c614272842705abd1c6a541
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07501410B2

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