2,4-Dichloro-3-ethyl-6-nitrophenol → Phenol, 6-amino-2,4-dichloro-3-ethyl-, hydrochloride (1:1)

525 ml of isopropyl alcohol, 125 g of the same 2-nitro-4,6-dichloro-5-ethylphenol as described above in (1) and 7.5 g of Raney nickel were placed in 1 liter of autoclave, and then the mixture was stirred until absorbing the theoretical amount of hydrogen gas under 10 kg/cm2 of initial pressure of hydrogen at 50° C. or less. Raney nickel catalysts were removed by filtration from the reaction mixture, and 165 g of concentrated hydrochloric acid was added to the resulting filtrate. Then, the resulting solution was stirred for 30 minutes at 40° to 50° C. to obtain white crystalline precipitates. Thereafter, the resulting crystal was cooled for 1 hour at 5° C. or less, and separated out, washed with 140 ml of acetone and dried to obtain 2-amino-4,6-dichloro-5-ethylphenol.hydrochloride. Yield was 112.5 g (87.5%).

1. customuntil absorbing the theoretical amount of hydrogen gas under 10 kg/cm2 of initial pressure of hydrogen at 50° C. or less
2. customRaney nickel catalysts were removed by filtration from the reaction mixture, and 165 g of concentrated hydrochloric acid
3. additionwas added to the resulting filtrate
4. stirringThen, the resulting solution was stirred for 30 minutes at 40° to 50° C.
5. customto obtain white crystalline precipitates
6. temperatureThereafter, the resulting crystal was cooled for 1 hour at 5° C. or less
7. customseparated out
8. washwashed with 140 ml of acetone
9. customdried

ORD-Eintrag

ord-a5d60f6518044b008e9086f16febeedf

Quelldatensatz

uspto-grants-1987_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04686177