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ChemicalBook CAS DataBase List Cyclopentyl chloroformate
50715-28-1

Cyclopentyl chloroformate synthesis

4synthesis methods
-

Yield:50715-28-1 97.4%

Reaction Conditions:

with triethylamine in dichloromethane at -5 - 20; for 13 h;

Steps:

11 Example 1
General procedure: In a jacketed reactor equipped with a mechanical stirrer, a thermometer, a constant pressure dropping funnel and an exhaust gas absorber,Add 7L dichloromethane, the first reaction phase, temperature -5 ° C,780 g (5 mol) of L-menthol and 1187 g (4 mol) of triphosgene were added in portions and sufficiently stirred to dissolve them.-5 ° CDrop under the drop1215 g (12mo 1) triethylamine in methylene chloride (1.8 L) was added dropwise over 1 to 2 h,Insulation reaction 3h after the natural temperature rise to the second reaction stage, temperature control 25 ° C, stirring about 10h.After completion of the reaction, the reaction mixture was separated by filtration under filtration, and the mother liquor was washed successively with 3 L of water, 3 L of dilute hydrochloric acid (5%), 0.5 L of sodium carbonate (5%) and 0.5 L of saturated brine ,After drying over anhydrous sodium sulfate, the solvent was removed by steaming and distilled under reduced pressure to collect 108 to 109 ° C / 1 ImmHg fraction,1063 g of a colorless liquid was obtained in a yield of 97.2%.

References:

Yangtze University;WU, Ai-bin;QIN, Shao-xiong;LI, Peng-Fei;GUO, Quanjing;HU, Bao-jun CN106045802, 2016, A Location in patent:Paragraph 0044-0045

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