3,3-dimethylphthalide synthesis
- Product Name:3,3-dimethylphthalide
- CAS Number:1689-09-4
- Molecular formula:C10H10O2
- Molecular Weight:162.19
Yield: 211 g
Reaction Conditions:
Stage #1:methyl bromide with iodine;magnesium in tetrahydrofuran for 2 h;Reflux;
Stage #2:phthalic anhydride in tetrahydrofuran at 20; for 2 h;
Steps:
1 Preparation of intermediate (3):
135 g of magnesium turnings, 750 mL of anhydrous tetrahydrofuran and 3 iodines were added to the reaction flask, slightly heated, 20 g of methyl bromide was added, the addition was completed, the temperature was refluxed for 2 h, and cooled to room temperature to obtain methyl bromide. Magnesium tetrahydrofuran format reagent was used; 300 g of phthalic anhydride (2) was added to the above solution, stirred at room temperature for 2 hours, 700 mL of water was added, the organic phase was separated, and the aqueous phase was extracted with 350 mL of dichloromethane, and the organic phase was combined. % sodium hydroxide solution is washed with water, and the organic layer is separated.Drying over anhydrous magnesium sulfate and concentrating to dryness afforded 211 g of Compound (3).
References:
Liaoning Bo Mei Pharmaceutical Technology Co., Ltd.;Wang Yan;Liu Yong;Li Wei;Jin Jian;Jiang Yu CN109824493, 2019, A Location in patent:Paragraph 0021; 0022
201230-82-2
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