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With ethanol; potassium hydroxide for 1h; Reflux; Large scale;
3.3 3. Hydrolysis reaction
1 kg of compound 3 was added to a solution of potassium hydroxide in ethanol (1010 g of potassium hydroxide, 7.3 L of ethanol) at room temperature, and the mixture was heated to reflux for 1 hour, and detected by TLC. After the reaction was completed, the reaction mixture was concentrated, and 5 L of water was added. The pH of the hydrochloric acid was adjusted to 2, ethyl acetate was evaporated, and the organic phase was combined, washed with brine, dried over sodium sulfate, and concentrated to afford 740 g of compound 4 (3-oxetanecarboxylic acid), yield 83.7%.
With acetic acid In methanol; dichloromethane at 0 - 20℃;
112.1
[0606] Step 1: [0607] At 0 °C, oxetane-3-carboxylic acid 81 (1.3 g, 12.73 mmol) was dissolved in a mixture of methanol (10 mL) and dichloromethane (10 mL), and trimethylsilyldiazomethane (2 M, 12.73 mL, 25.46 mmol) was slowly added. After the dropwise addition, the mixture was warmed to room temperature and stirred for 3 h. After the reaction was completed, acetic acid (0.05 mL) was added to the reaction mixture. The mixture was poured into water, and extracted with dichloromethane (2330 mL). The organic phases were combined, and dried with anhydrous sodium sulfate. The mixture was filtered, and the filtrate was concentrated under reduced pressure to afford crude compound 82 (1.4 g, yield: 94.7%) as a colorless oil.
94.7 %
With acetic acid In methanol; dichloromethane at 0 - 20℃;
112.1
[0606] Step 1: [0607] At 0 °C, oxetane-3-carboxylic acid 81 (1.3 g, 12.73 mmol) was dissolved in a mixture of methanol (10 mL) and dichloromethane (10 mL), and trimethylsilyldiazomethane (2 M, 12.73 mL, 25.46 mmol) was slowly added. After the dropwise addition, the mixture was warmed to room temperature and stirred for 3 h. After the reaction was completed, acetic acid (0.05 mL) was added to the reaction mixture. The mixture was poured into water, and extracted with dichloromethane (2330 mL). The organic phases were combined, and dried with anhydrous sodium sulfate. The mixture was filtered, and the filtrate was concentrated under reduced pressure to afford crude compound 82 (1.4 g, yield: 94.7%) as a colorless oil.
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