2,6-Dichloroaniline → (2,6-Dichlorophenyl)hydrazine monohydrochloride

温度

5 °C

To a cold solution of 2,6-dichloroaniline (10.0 g, 61.72 mmol) in conc. HCl was added aqueous solution of sodium nitrite (5.11 g, 74.00 mmol) at −15° C. The reaction mass was stirred at 0-10° C. for 15 minutes. The reaction mass was filtered off to remove insolubles and stannous chloride in conc. HCl (34.7 g, 150 mmol) was added to the filtrate. The reaction mass was further stirred at −15° C. for 30 min and filtered to afford 15.00 g of the desired product. 1H NMR (300 MHz, DMSO d6): δ 7.18-7.28 (m, 1H), 7.39-7.52 (m, 2H), 10.30 (br s, 3H); MS (m/z): 176.90 (M)+.

1. filtrationThe reaction mass was filtered off
2. additionwas added to the filtrate
3. stirringThe reaction mass was further stirred at −15° C. for 30 min
4. filtrationfiltered

ORDレコード

ord-87c73f6492094632b7e5a271243807e2

出典データセット

uspto-grants-2015_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09096545B2