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ChemicalBook CAS DataBase List 1,7-Heptanediol

1,7-Heptanediol synthesis

10synthesis methods
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Yield:629-30-1 95.3%

Reaction Conditions:

with lithium aluminium tetrahydride in tetrahydrofuran at 5 - 20; for 2.5 h;Large scale;

Steps:

3.2 Example 3
(2) Synthesis of 1,7-heptanediol
Add 25000 ml of tetrahydrofuran to a 50-liter glass reactor and start stirring.Add 1500g lithium tetrahydroaluminate when cooling to 5°C,Then, a mixture of 5000 g of dimethyl pimelate and 5000 ml of tetrahydrofuran was transferred to a dropping funnel.When the temperature of the reaction flask dropped to 5°C, it began to be added dropwise.Control the temperature at 5 °C, after the completion of the drop 1hThe mixture was slowly heated to room temperature and stirred for 1.5 hours. After the sample was taken, no raw material remained. It was qualified. The temperature was lowered to 5° C., and 1500 g of water, 1500 g of 15% sodium hydroxide solution, and 1500 g of water were added dropwise. The filtrate was concentrated to give 3360 g 1, Crude 7-heptanediol, crude 1,7-heptanediol was distilled under reduced pressure by an oil pump, and the oil bath temperature was 105°C.The gas-phase collection temperature is 74°C, giving 3201 g of 1,7-heptanediol,Content 99.6%, yield 95.3%;

References:

Haimen Huaxiang Pharmaceutical Technology Co., Ltd.;Wu Tiansheng;Zhou Guang;Xu Benquan CN107417496, 2017, A Location in patent:Paragraph 0012; 0013; 0014

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