Ammonium Chloride → HCID 84665992, 화합물

HRID 2208918노트

반응식

HRID 2208918 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([N+:14]([O-])=O)[C:6]([CH3:13])=[C:7]([CH:12]=1)[C:8]([O:10][CH3:11])=[O:9].[Cl-].[NH4+]>C(O)C.O.[Fe]>[NH2:14][C:5]1[C:6]([CH3:13])=[C:7]([CH:12]=[C:3]([O:2][CH3:1])[CH:4]=1)[C:8]([O:10][CH3:11])=[O:9]

참가 물질

6

반응물 2

HCID 25517Ammonium ChlorideHCID 53399479Benzoic acid, 5-methoxy-2-methyl-3-nitro-, methyl ester

생성물 1

HCID 84665992HCID 84665992, 화합물수율 80.9%

시약·촉매·용매 3

HCID 23925Iron촉매HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

To a stirred solution of methyl 5-methoxy-2-methyl-3-nitrobenzoate (1.7 g, 7.6 mmol) in ethanol (20 mL) was added ammonium chloride (1.7 g, 32 mmol) dissolved in water (20 mL) and iron powder (3.38 g, 60.44 mmol). The mixture was heated at 80° C. for 3 h, filtered and the residue washed well with hot ethanol. The filtrate was concentrated and the residue was basified with aqueous sodium bicarbonate. The aqueous phase was extracted with ethyl acetate. The combined organic layers were washed with water, dried, and concentrated under reduced pressure to give the crude title compound (1.2 g) which was used directly in the next step.

후처리

  1. filtrationfiltered
  2. washthe residue washed well with hot ethanol
  3. concentrationThe filtrate was concentrated
  4. extractionThe aqueous phase was extracted with ethyl acetate
  5. washThe combined organic layers were washed with water
  6. customdried
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-4eeb3cc9326e4c23b233baf73eaf3899
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09376422B2

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