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4-Methylphthalimide → 5-Methyl-2,3-dihydro-1H-isoindol-1-one

HRID 1811009
ノート
印刷プレビュー

反応式

HRID 1811009 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[C:7](=[O:11])[NH:6][C:5]2=O.[Sn]>C(O)(=O)C.Cl>[CH3:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[C:7](=[O:11])[NH:6][CH2:5]2
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 51482694-MethylphthalimideHCID 5352426Tin atom

生成物 1

HCID 220646715-Methyl-2,3-dihydro-1H-isoindol-1-one収率 50.4%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 313Hydrochloric Acid溶媒

実験手順

Step 1 A mixture of 5-methylisoindoline-1,3-dione (5.00 g, 31.0 mmol) and tin shavings (8.84 g, 74.5 mmol) in acetic acid (30 mL) and concentrated hydrochloric acid (15 mL) was heated at reflux for 3 h. The hot solution was filtered and the residual tin shavings were washed with acetic acid. The filtrate was concentrated and the residue was diluted with DCM (200 mL), and washed with water (20 mL) and brine (20 mL), dried and concentrated. The precipitate which formed during the concentration was collected by filtration and washed with DCM (5 mL) and dried under vacuum to give 5-methylisoindolin-1-one (2.3 g, 50%). 1H NMR (400 MHz, chloroform-d) δ 7.70 (1 H, d, J=7.77 Hz), 7.43 (1 H, s), 7.35 (1 H, d, J=7.77 Hz), 4.46 (2 H, s), 2.48 (3 H, s). Mass spectrum m/z 148.0 (M+H)+.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 3 h
  3. filtrationThe hot solution was filtered
  4. washthe residual tin shavings were washed with acetic acid
  5. concentrationThe filtrate was concentrated
  6. additionthe residue was diluted with DCM (200 mL)
  7. washwashed with water (20 mL) and brine (20 mL)
  8. customdried
  9. concentrationconcentrated
  10. customThe precipitate which formed during the concentration
  11. filtrationwas collected by filtration
  12. washwashed with DCM (5 mL)
  13. customdried under vacuum

出典と根拠

ORDレコード
ord-dd2204e6ccc8440b80473a64e7f430f1
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08362065B2

反応ノート

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