反応 #1833258

反応方程式

sodium hydroxide

methyl 4-amino-6-(benzo[d][1,3]dioxol-4-yl)-3-chloro-5-fluoropicolinate

HCl

→

title compound

収率 74.6%

4-Amino-6-(benzo[d][1,3]dioxol-4-yl)-3-chloro-5-fluoropicolinic acid

収率 74.6%

溶媒

methanol

反応条件

後処理

1. 1
   濃縮concentrated under a stream of nitrogen
2. 2
   その他The precipitate that formed
3. 3
   ろ過was filtered off
4. 4
   洗浄washed with water
5. 5
   その他dried

実験手順

To a reaction vessel containing methyl 4-amino-6-(benzo[d][1,3]dioxol-4-yl)-3-chloro-5-fluoropicolinate (0.150 g, 0.462 mmol) was added methanol (9.24 mL) and 2 N sodium hydroxide (0.924 mL, 1.848 mmol). The reaction mixture was stirred overnight at room temperature, neutralized to pH 3 with 2 N HCl, and concentrated under a stream of nitrogen. The precipitate that formed was filtered off, washed with water, and dried to provide the title compound as a white solid (0.107 g, 74.6%): mp 171-173° C.; 1H NMR (400 MHz, DMSO-d6) δ 7.08-7.00 (m, 2H), 6.99-6.93 (m, 2H), 6.93 (br s, 2H), 6.06 (s, 2H); ESIMS m/z 311.2 ([M+H]+), 309.1 ([M−H]−).

出典