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

HRID 1811009
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HRID 1811009 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 51482694-MethylphthalimideHCID 5352426Tin atom

생성물 1

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

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 313Hydrochloric Acid용매

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-dd2204e6ccc8440b80473a64e7f430f1
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08362065B2

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