Hydrochloric Acid → 3-Bromo-5-chlorotoluene

温度

0 °C

Step G1. To an ice-water-cooled and stirred solution of 2-amino-5-bromo-3-chlorotoluene (12 g, 54 mmol) in a mixture of 100 mL of acetic acid, 43 mL of H2O and 11.5 mL of concentrated HCl was added dropwise a solution of NaNO2 (4.48 g, 65 mmol) in 15 mL of H2O. The reaction mixture was stirred for 30 min and was then added to an 112 mL solution of 50% H3PO2 cooled at 0° C. After being stirred for 6 h at 0° C., the reaction mixture was allowed to stand at room temperature overnight. The solid was filtered and washed with water, then dried in vacuum. 3-Chloro-5-bromo-toluene (9 g, 81%) was obtained as brown solid. Crystals. 1H NMR (CDCl3): δ 2.31 (s, 3H), 7.10 (s, 1H), 7.21 (s, 1H), 7.31 (s, 1H).

1. stirringAfter being stirred for 6 h at 0° C.
2. waitto stand at room temperature overnight
3. filtrationThe solid was filtered
4. washwashed with water
5. customdried in vacuum

ORDレコード

ord-8b70b921f7cf4718b4ea13c1719f3c02

出典データセット

uspto-grants-2007_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07273882B2