ChemicalBook CAS DataBase List 3-Bromo-2,2-bis(bromomethyl)propanol

3-Bromo-2,2-bis(bromomethyl)propanol synthesis

5synthesis methods

Product Name:3-Bromo-2,2-bis(bromomethyl)propanol
CAS Number:1522-92-5
Molecular formula:C5H9Br3O
Molecular Weight:324.84

3-broMo-2,2-bis(broMoMethyl)propyl acetate

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Yield:1522-92-5 93%

Reaction Conditions:

with methanol at 80; for 2 h;

Steps:

1-4 Example 3:A preparation method of tribromoneopentyl alcohol includes the following steps:
add 272.3g (2.0mol, 1.0eq) of pentaerythritol, 48.1g (1.5 mol, 0.75eq) sulfur powder and 1361.5g (22.67mol, 11.34eq) acetic acid, 639.2g (4.0mol, 2.0eq) liquid bromine was added dropwise with stirring, and the internal temperature was controlled not to exceed 50 ° C. Then slowly raise the temperature to 120 ° C and continue stirring for 6h to end the reaction. The conversion rate of tribromoneopentyl alcohol reaches more than 90%, and the temperature is reduced to 80 ° C. Acetic acid and hydrobromic acid are recovered by distillation under reduced pressure at -0.09MPa. 975 mL of methanol was added to the residue, alcoholysis was carried out at 80 ° C for 2 hours, and methanol and methyl acetate were recovered by distillation under reduced pressure. The residue was cooled to 50 ° C, 1000 mL of water was added to the reaction system, the pH of the system was adjusted to 7.0 to 8.0 with a 10% sodium carbonate aqueous solution, and the mixture was kept under stirring at 50 ° C for 30 minutes, cooled to 50 ° C, and 585 mL of n-pentane was added to the system , Stir for 30 minutes and separate. The organic phase was cooled to 0 ° C, a large amount of white crystals were precipitated, filtered with suction, and dried at 50 ° C for 6 hours to obtain 604.2 g of tribromoneopentyl alcohol with a yield of 93% and a purity of 99.6% (GC).

References:

Cong Qiang;Li Wan CN110903163, 2020, A Location in patent:Paragraph 0010; 0023-0030

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