3-Methyl-2-nitroanisole → 2-Methoxy-6-methylaniline

HRID 1389506

반응식

HRID 1389506 반응식
[N+:1]([C:4]1[C:9]([CH3:10])=[CH:8][CH:7]=[CH:6][C:5]=1[O:11][CH3:12])([O-])=O>C(O)(=O)C.[Fe]>[CH3:12][O:11][C:5]1[CH:6]=[CH:7][CH:8]=[C:9]([CH3:10])[C:4]=1[NH2:1]

참가 물질

4

반응물 1

HCID 792913-Methyl-2-nitroanisole

생성물 1

HCID 4592492-Methoxy-6-methylaniline

시약·촉매·용매 2

HCID 23925Iron촉매HCID 176Acetic Acid용매

실험 절차

Solid 2-nitro-3-methylanisole (20 g) is added portion to a hot (40°-60° C.) suspension of iron (30 g) in 20% acetic acid (400 ml). The mixture is heated on a steam bath for 40 min, filtered still hot and neutralized (after cooling) with 50% aqueous sodium hydroxide. The mixture is steam distilled (2 liters of water collected). The distillate is extracted with diethyl ether and the etheral solution is dried and evaporated to give an oily residue of 2-methoxy-6-methylbenzenamine: nmr (CDCl3) δ2.15 (s, 3H), 3.7 (s, 2H), 3.8 (s, 3H) and 6.7 (m, 3H).

후처리

  1. temperatureThe mixture is heated on a steam bath for 40 min
  2. filtrationfiltered still hot
  3. temperatureneutralized (after cooling) with 50% aqueous sodium hydroxide
  4. distillationdistilled
  5. custom(2 liters of water collected)
  6. extractionThe distillate is extracted with diethyl ether
  7. customthe etheral solution is dried
  8. customevaporated

출처 및 근거

ORD 기록
ord-d7378ab606ba4a589d1d7b2258d3be89
출처 데이터셋
uspto-grants-1981_01
특허 번호
US04244966

연결된 노트

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