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ChemicalBook CAS DataBase List 2-Bromo-3,3,3-trifluoropropan-1-ol
311-86-4

2-Bromo-3,3,3-trifluoropropan-1-ol synthesis

3synthesis methods
-

Yield: 90.2%

Reaction Conditions:

Stage #1:1,1,1-trifluoropropylene with N-Bromosuccinimide;sulfuric acid;acetic acid at 80 - 100; for 4 h;
Stage #2: in methanol at 40; for 9 h;

Steps:

Preparation of 2 - bromo - 3,3,3 - trifluoropropanol as starting material
4.0mol of glacial acetic acid was added to the reaction flask, and the temperature was increased to 90 ° C with stirring. 0.4mol of NBS and 6.4g of concentrated sulfuric acid were added, and 3,3,3-trifluoropropene was introduced at the same time. After the reaction system was clarified, 0.20mol of NBS and 3.2 G of concentrated sulfuric acid, the reaction system clarified, then add 0.40molNBS and 6.4g concentrated sulfuric acid, the reaction system clarified, 80C reaction 2h, temperature to 100C to continue the reaction 2h, 3,3,3-trifluoropropene into the 1.3mol . Cooling to 40 ° C, adding 7mol methanol stirring under reflux, the reaction 9h. Methanol and methyl acetate were distilled off at normal pressure. After cooling, the solid was filtered off, and 2-bromo-3,3,3-trifluoropropanol was obtained by distillation under reduced pressure. The yield was 90.2% and the content was 99.1%.

References:

Xi'an Modern Chemistry Research Institute;Gu, Yujie;Lu, Jian;Ma, Hui;Wang, Zhixuan;Kang, Jianping;Du, Yongmei;Tu, Donghuai;Wan, Hong;Li, Yang CN105399607, 2016, A Location in patent:Paragraph 0014; 0015