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ChemicalBook CAS DataBase List 6-Chlorohexanol
2009-83-8

6-Chlorohexanol synthesis

10synthesis methods
6-Chlorohexanol is obtained from the reaction of 1,6-Hexanediol with hydrochloric acid.
-

Yield:2009-83-8 95.2%

Reaction Conditions:

with 1,3,5-trichloro-2,4,6-triazine in N,N-dimethyl-formamide at -5 - 0; for 2 h;Large scale;Solvent;Temperature;

Steps:

1-3; 1-4

1) Add 3.7kg DMF to the four-neck bottle,Stir, the temperature is controlled at 10-20,Add 738g of cyanuric chloride in batches,After adding, stir for 6h,The detection of cyanuric chloride has been completed.
2) Prepare 473g 1,6-hexanediolAnd 500g of DMF mixed solution,Stir, control the temperature at -5-0,Drop the reaction solution prepared in 1), after the addition is complete,Stir and react for 2 hours at 0°C,Stop refrigeration and naturally heat up to 25°C,Sampling and control, when 1,6-hexanediol is completely reacted, the reaction is over.
3) The mixed reaction liquid obtained in step 3) is filtered under low vacuum,The filter cake is rinsed with 100g of DMF,Drain and combine the DMF solution of the product.
4) Vacuum distillation product, control the vacuum degree at 5mmHg,Slowly heat up and rectify,Obtained product: 520 g, purity 99.52%: yield: 95.2%.The GC spectrum and H-NMR of the product obtained in this example are shown in Figure 1-2, respectively.

References:

CN112239395,2021,A Location in patent:Paragraph 0035-0062

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