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Methyl iodide → 7-Methylsulfanyl-2-isopropyl-4-bromo-2H-phthalazin-1-one

HRID 1765348
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반응식

HRID 1765348 반응식
[SH:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([Br:16])=[N:7][N:8]([CH:13]([CH3:15])[CH3:14])[C:9]2=[O:12])=[CH:4][CH:3]=1.[H-].[Na+].[CH3:19]I>O1CCCC1>[CH3:19][S:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([Br:16])=[N:7][N:8]([CH:13]([CH3:14])[CH3:15])[C:9]2=[O:12])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 1363729987-Mercapto-2-isopropyl-4-bromo-2H-phthalazin-1-one

생성물 1

HCID 211065857-Methylsulfanyl-2-isopropyl-4-bromo-2H-phthalazin-1-one수율 54%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 7-Mercapto-2-isopropyl-4-bromo-2H-phthalazin-1-one (0.77 g, 2.6 mmol) in tetrahydrofuran (THF) (8 ml), was added NaH (60%, 0.13 g, 3.1 mmol) portion-wise. After stirring for five minutes, methyl iodide (0.44 g, 3.1 mmol) was added dropwise and stirring was continued for four hours. The mixture was concentrated under vacuum and the residue was subjected to flash column chromatography (elution: 90% heptane, 10% ethyl acetate) to give the title compound (0.44 g, 54% yield) as a white solid.

후처리

  1. stirringstirring
  2. waitwas continued for four hours
  3. concentrationThe mixture was concentrated under vacuum
  4. washthe residue was subjected to flash column chromatography (elution: 90% heptane, 10% ethyl acetate)

출처 및 근거

ORD 기록
ord-51308b2ba9cb46c89bf12f488347e741
출처 데이터셋
uspto-grants-2007_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07226923B2

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