Methylamine → 6-bromo-2-methyl-2,3-dihydro-1H-isoindol-1-one

HRID 82048

반응식

HRID 82048 반응식
C[O:2][C:3](=O)[C:4]1[CH:9]=[C:8]([Br:10])[CH:7]=[CH:6][C:5]=1[CH2:11]Br.[CH3:14][NH2:15]>C1COCC1>[Br:10][C:8]1[CH:9]=[C:4]2[C:5]([CH2:11][N:15]([CH3:14])[C:3]2=[O:2])=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 12929136Methyl 5-bromo-2-(bromomethyl)benzoate

생성물 1

HCID 469420086-bromo-2-methyl-2,3-dihydro-1H-isoindol-1-one수율 100%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
50 °C

실험 절차

To a solution of 5-bromo-2-bromomethyl-benzoic acid methyl ester (1.00 g, 3.25 mmol) in THF (6.5 mL) was a solution of methylamine in THF (2M, 8.12 mL, 16.24 mmol). The reaction mixture was heated at 50° C. for 4 hours and then concentrated under vacuum. The residue was taken up in EtOAc and the organic layer was then washed with an aqueous 1M HCl solution, brine, dried (Na2SO4), filtered, concentrated under vacuum to give the title compound (0.73 g, 100%) as a yellow solid.

후처리

  1. concentrationconcentrated under vacuum
  2. washthe organic layer was then washed with an aqueous 1M HCl solution, brine
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-6e174c0561454a2d8fc1dd1e6727ca38
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846712B2

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