Water → 4-Chloro-5-methoxy-2-nitro-phenylamine

HRID 408695노트

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HRID 408695 반응식
[Cl:1][C:2]1[C:7](Cl)=[CH:6][C:5]([NH2:9])=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=1.[CH3:13][O-:14].[Na+].O>CO>[Cl:1][C:2]1[C:7]([O:14][CH3:13])=[CH:6][C:5]([NH2:9])=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 811494,5-Dichloro-2-nitroanilineHCID 10942334Sodium Methoxide

생성물 1

HCID 203767444-Chloro-5-methoxy-2-nitro-phenylamine수율 56%

시약·촉매·용매 1

HCID 887Methanol용매2회

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온도
100 °C

실험 절차

To a mixture of 4,5-dichloro-2-nitro-phenylamine (1.29 g, 6.23 mmol) and dry MeOH (2 mL), a 25 wt % solution of sodium methoxide in MeOH (10 mL) was added and the mixture stirred for 6 h at 100° C. in a sealed tube. The mixture was cooled to 23° C., poured into water (50 mL), and extracted with EtOAc (3×50 mL). The combined organic layers were washed with brine (25 mL), dried, filtered, and concentrated under reduced pressure to afford the titled compound (0.700 g, 56%). The crude material was used without further purification in the next reaction.

후처리

  1. temperatureThe mixture was cooled to 23° C.
  2. extractionextracted with EtOAc (3×50 mL)
  3. washThe combined organic layers were washed with brine (25 mL)
  4. customdried
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-672c580f1ebb4242874e1b64d5ae7e04
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08759345B2

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