
4-METHYLPHTHALIMIDE 99 synthesis
- Product Name:4-METHYLPHTHALIMIDE 99
- CAS Number:40314-06-5
- Molecular formula:C9H7NO2
- Molecular Weight:161.16

19438-61-0

40314-06-5
General procedure for the synthesis of 4-methylphthalimide from 5-methylisobenzofuran-1,3-dione (Intermediate Example 71): 5-methyl-2,3-dihydro-1H-isoindole xylene (15 mL) was added to a reaction vial containing 4-methylphthalic anhydride (3.0 g) and urea (1.2 g). The reaction mixture was stirred at 150°C overnight. After completion of the reaction, the mixture was cooled to room temperature and the precipitated crystals were collected by filtration and washed sequentially with ethanol and water. The resulting crystals were dried under reduced pressure to give 4-methylphthalimide (2.4 g, 82% yield) as white crystals.1H NMR (CDCl3) δ (ppm): 2.5 (3H, s), 7.5 (1H, d), 7.6 (1H, s), 7.7 (1H, s).

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Yield: 85%
Reaction Conditions:
with manganese(IV) oxide;ammonium hydroxide;oxygen;chlorobenzene in N,N-dimethyl-formamide at 100; under 15001.5 Torr; for 24 h;Autoclave;Green chemistry;
Steps:
6; 30 Example 30:
General procedure: 0.01g of MnO2 catalyst, 0.5mmol of 1-indanone, 0.2g of ammonia water (25wt%) and 2g of chlorobenzene were added to a stainless steel autoclave with a polytetrafluoroethylene inner liner.The temperature was raised to 110 by automatic temperature controller, 0.6MPa oxygen was added and the reaction was continued for 4h. The pressure was kept constant during the reaction.The reaction product was analyzed using GC-MS with a phthalamide yield of 85%.
References:
Dalian Institute of Chemical Physics;Wang Feng;Wang Min;Xu Jie;Ma Jiping;Yu Miao;Zhang Xiaochen;Zhang Zhe CN106278990, 2017, A Location in patent:Paragraph 0013; 0017; 0018; 0020; 0023; 0028

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