1-ブロモ-2,3-ジフルオロベンゼン 化学特性,用途語,生産方法
外観
無色～ほとんど無色透明液体
化学的特性
Clear colorless to peach liquid
使用
1-Bromo-2,3-difluorobenzene may be used in the synthesis of potent, orally active Calcitonin gene-related peptide (CGRP) receptor antagonist (BMS-846372). It may be used in the preparation of 2,3-difluorophenyl(dimethyl)phosphane.
一般的な説明
Microbial oxidation of 1-bromo-2,3-difluorobenzene by
Pseudomonas putida strain 39/D and
Escherichia coli recombinant microorganism (strain JM 109(pDTG601)) has been reported.
合成
Add
50% aqueous solution of KOH (18.0 g, 160 mmol) to a mixture of
1-bromo-5,5,6,6-tetrafluorocyclohex-1-ene (11.65 g) and
triethylbenzylammonium chloride (0.15 g, 0.7 mmol) at 30-35°C for 30
minutes. Keep the reaction mixture at 75-85°C for 2 hours. Cool the
reaction mixture. Dilute the reaction mixture with water. Extract the
organic product with CH2Cl2. Dry the organic product over CaCl2. Distill the organic product. 1H NMR (CDCl3, 300.1 MHz), δ: 7.00-7.16 (m, 1H, Ar); 7.17-7.29 (m, 1H, Ar); 7.34-7.47 (m, 1H, Ar). 13C NMR (CDCl3,
75.5 MHz), δ: 110.40 (d, C(1), J = 17.5 Hz); 116.40 (d, C(4), J = 17.7
Hz); 124.70 (dd, C(5), J = 7.1 Hz, J = 5.0 Hz); 128.23 (d, C(6), J = 3.6
Hz); 148.10 (dd, C(2), J = 248.8 Hz, J = 14.3 Hz); 150.92 (dd, C(3), J =
251.9 Hz, J = 13.3 Hz). 19F NMR (CDCl3, 282.4 MHz), δ: -130.9 (m, 1 F, Ar), -134.8 (m, 1 F, Ar). BP 157-158°C. Elemental Analysis Found (%): C, 37.54; H, 1.50. C6H3BrF2. Calculated (%): C, 37.34; H, 1.52. Mass Spec MS, m/z (Irel (%)): 194, 192 [M]+ (100, 99), 113 [M-Br]+ (88), 63 (60).
Fig The synthetic method of 1-Bromo-2,3-difluorobenzene
貯蔵
Keep container sealed and store in an ventilated, low temperature, dry warehouse, separate from foods and oxidizing agents.
1-ブロモ-2,3-ジフルオロベンゼン 上流と下流の製品情報
原材料
準備製品