天堂网亚洲,天天操天天搞,91视频高清,菠萝蜜视频在线观看入口,美女视频性感美女视频,95丝袜美女视频国产,超高清美女视频图片

Welcome to chemicalbook!
Chinese English Japanese Germany Korea
400-158-6606
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

ChemicalBook CAS DataBase List Methyl 3-amino-5-bromobenzoate
706791-83-5

Methyl 3-amino-5-bromobenzoate synthesis

5synthesis methods
3-Bromo-5-aminobenzoic acid (1.0 g, 4.62 mmol) was stirred in methanol (15mL) with ice cooling, and the yellow solution was treated with thionyl chloride (4.00 mL, 55.0 mmol) dropwise over 20 mm. The resulting mixture was allowed to warm to room temperature and left stirring overnight. The reaction mixture was quenched with aqueous saturated NaHCO3 solution at 0 C. The solvent was then removed under vacuum, and the residue was suspended in ethyl acetate (200 mL). The organic phase was washed with brine (100 mL), dried (Na2504) and concentrated to afford Methyl 3-amino-5-bromobenzoate as a yellow solid (1.08 g, 98%). NMR (400 MHz, Methanol-d) oe 7.10 (t, J 1.6 Hz, 1H), 6.83 (t, J 1.6 Hz, 1H), 6.57 (t, J= 1.6 Hz, 1H), 3.46 (s, 3H). 13C NMR (100 MHz, CDC13) oe: 52.3, 114.6, 121.6, 122.3, 122.9, 132.6, 147.7, 166.0. m/z (ESI, MH) 231.
-

Yield:-

Steps:

Multi-step reaction with 3 steps
1: sulfuric acid; N-Bromosuccinimide / 2 h / 60 °C
2: sodium carbonate / N,N-dimethyl-formamide / 8 h / 60 °C
3: ammonium chloride; iron / ethanol; water / 1 h / 80 °C

References:

Kuntz, Kevin W.;Campbell, John E.;Keilhack, Heike;Pollock, Roy M.;Knutson, Sarah K.;Porter-Scott, Margaret;Richon, Victoria M.;Sneeringer, Chris J.;Wigle, Tim J.;Allain, Christina J.;Majer, Christina R.;Moyer, Mikel P.;Copeland, Robert A.;Chesworth, Richard [Journal of Medicinal Chemistry,2016,vol. 59,# 4,p. 1556 - 1564]

Methyl 3-amino-5-bromobenzoate Related Search: