纯度：95%
货期：4-5周
质量要求：无无机盐残留，HNMR无明显杂峰，HPLC>95%
基本信息
- 英文名称：
- 2,5-bis(trifluoromethyl)terephthalic acid
- 英文别名：
- 1,4-Benzenedicarboxylic acid,2,5-bis(trifluoromethyl);
2,5-ditrifluoromethylterephthalic acid;
H2BDC-(CF3)2;
- CAS号：
- 366008-67-5
- 分子式：
- C10H4F6O4
- 分子量：
- 302.12700
- 精确质量：
- 302.00100
- PSA：
- 74.60000
- LogP：
- 3.12060
参考路线：
2,5-diperfluoroterephthalic acid was synthesized in two steps according to the reported method. 2
19 g (88,7 mmol ) of 1,4-bis(trifluoromethyl)benzene, 250 mL of trifluoroacetic acid (SDS) and 60
mL of sulfuric acid (95-98%; Acros) were stirred under reflux for 10 min. Then, 47.4 g (267 mmol) of
N-bromosuccinimide (Aldrich) were slowly added during 5 h and maintained at 60°C under stirring for
48 h. The 2,5-dibromo-1,4-bis(trifluoromethyl)benzene was precipitated by addition of ice (500 g) to the
crude mixture, filtered and dried under vacuum (1 mm Hg) for 24 h. The product was purified by
sublimation to obtain 91% of a white solid.
Melting point: 65 ± 0.2°C ; RMN
1 H (200 MHz, CDCl 3 ) : 8,01 (2H, s) ; RMN 19 F (188 MHz,
CDCl 3 ) : -64,1 (2 X CF 3 , s).
16 g (43 mmol) of 2,5-dibromo-1,4-bis(trifluoromethyl)benzene in 100 mL of THF was added dropwise
to a solution of 38.4 mL (67,2 mmol) of butyllithium (2,5 M in hexane) in 75 mL of THF cooled to 6-
78°C. After 30 min. of stirring at this temperature, 200 g of crushed dry ice was added. After coming to
ambient temperature, the mixture was extracted three times by 100 mL of a solution of sodium
hydroxide (2M). The aqueous phases were acidified by a solution of hydrochloric acid (2M) and the
precipitate formed was filtered and dried under vacuum (1 mm Hg) for 24 h to give 11 g (84%) of 2,5-
ditrifluoromethylterephthalic acid as a white solid.
