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Sodium Hydroxide → 4-Methyl-3-(1-methylphthalazin-6-yl)benzoic acid

HRID 422550
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HRID 422550 반응식
[CH3:1][C:2]1[CH:12]=[CH:11][C:5]([C:6]([O:8]CC)=[O:7])=[CH:4][C:3]=1[C:13]1[CH:14]=[C:15]2[C:20](=[CH:21][CH:22]=1)[C:19]([CH3:23])=[N:18][N:17]=[CH:16]2.[OH-].[Na+]>O1CCCC1.CO>[CH3:1][C:2]1[CH:12]=[CH:11][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[C:13]1[CH:14]=[C:15]2[C:20](=[CH:21][CH:22]=1)[C:19]([CH3:23])=[N:18][N:17]=[CH:16]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 59726018Ethyl 4-methyl-3-(1-methylphthalazin-6-yl)benzoate

생성물 1

HCID 597260224-Methyl-3-(1-methylphthalazin-6-yl)benzoic acid

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of ethyl 4-methyl-3-(1-methylphthalazin-6-yl)benzoate (51.7 mg, 169 μmol) in tetrahydrofuran (800 μl) and methanol (400 μl) was added 1N aqueous sodium hydroxide solution (338 μl, 338 μmol) and stirred at RT for 18 h. The reaction was concentrated in vacuo and the residue was taken up in water and the pH was adjusted with 10% aqueous HCl solution to ˜7. The aqueous mixture was extracted with 15% MeOH/CHCl3 (3×) and the organic extracts were combined, dried (MgSO4), filtered, and concentrated in vacuo to give 4-methyl-3-(1-methylphthalazin-6-yl)benzoic acid as a maize solid. MS (ES+): 279.1 (M+H)+.

후처리

  1. concentrationThe reaction was concentrated in vacuo
  2. extractionThe aqueous mixture was extracted with 15% MeOH/CHCl3 (3×)
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-183274199dd54dd581858722a2eb47e7
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08101612B2

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