Hydrochloric Acid → 2-Amino-4-chloro-5-methylphenol

HRID 337366

반응식

HRID 337366 반응식
[Cl:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([OH:9])=[C:4]([N+:10]([O-])=O)[CH:3]=1.Cl.[Cl-].[NH4+]>CO.O.[Zn]>[NH2:10][C:4]1[CH:3]=[C:2]([Cl:1])[C:7]([CH3:8])=[CH:6][C:5]=1[OH:9]

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 235324-Chloro-5-methyl-2-nitrophenolHCID 25517Ammonium Chloride

생성물 1

HCID 1045242-Amino-4-chloro-5-methylphenol수율 33.3%

시약·촉매·용매 3

HCID 23994Zinc촉매HCID 887Methanol용매HCID 962Water용매

실험 절차

To a solution of 4-chloro-5-methyl-2-nitrophenol (5.0 g) in methanol (100 mL) at 0° C. was added zinc powder (8.71 g), which was activated by hydrochloric acid in advance, and a solution of ammonium chloride (7.1 g) in water (20 mL). The suspension was stirred for 4 h at room temperature. Then the insoluble material was filtered off through celite, and the celite cake was washed with ethyl acetate (100 mL). The filtrate and washings were combined and concentrated under reduced pressure. The residue was purified by column chromatography over silica gel using hexane/ethyl acetate (3:2) to yield the title compound (1.4 g).

후처리

  1. filtrationThen the insoluble material was filtered off through celite
  2. washthe celite cake was washed with ethyl acetate (100 mL)
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by column chromatography over silica gel

출처 및 근거

ORD 기록
ord-97d8b1235d82491fa0de0d796401146c
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08889727B2

연결된 노트

불러오는 중…