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

HRID 82048

反応式

HRID 82048 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
50 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6e174c0561454a2d8fc1dd1e6727ca38
出典データセット
uspto-grants-2014_09
特許番号
US08846712B2

関連ノート

読み込み中…