Water → 4-Chloro-2-fluoro-5-(pentyloxycarbonylmethyloxy)aniline

HRID 704090

반응식

HRID 704090 반응식
O.[Cl:2][C:3]1[C:8]([O:9][CH2:10][C:11]([O:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])=[O:12])=[CH:7][C:6]([N+:19]([O-])=O)=[C:5]([F:22])[CH:4]=1>C(O)(=O)C.[Fe]>[Cl:2][C:3]1[C:8]([O:9][CH2:10][C:11]([O:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])=[O:12])=[CH:7][C:6]([NH2:19])=[C:5]([F:22])[CH:4]=1

참가 물질

5

반응물 2

HCID 962WaterHCID 146178494-Chloro-2-fluoro-5-(pentyloxycarbonylmethyloxy)nitrobenzene

생성물 1

HCID 146178504-Chloro-2-fluoro-5-(pentyloxycarbonylmethyloxy)aniline수율 75.2%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 176Acetic Acid용매2회

반응 조건

온도
80 °C

실험 절차

A mixture of iron powders (115 g), acetic acid (29 g) and water (551 g) was heated at 80° C., and a solution of the compound (III) (132 g) in acetic acid (200 g) was dropwise added thereto in 1 hour, followed by heating under reflux for 5 hours. The reaction mixture was filtered to remove insoluble materials, and the filtrate was extracted with ethyl acetate. The extract was concentrated under reduced pressure. The residue was distilled off under reduced pressure to give 4-chloro-2-fluoro-5-(pentyloxycarbonylmethyloxy)aniline (Compound (II)) (90 g). Yield, 75%. b.p., 145°-149° C./0.4 mmHg. m.p., 32°-34° C.

후처리

  1. temperatureby heating
  2. temperatureunder reflux for 5 hours
  3. filtrationThe reaction mixture was filtered
  4. customto remove insoluble materials
  5. extractionthe filtrate was extracted with ethyl acetate
  6. concentrationThe extract was concentrated under reduced pressure
  7. distillationThe residue was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-3586a230fbe5452ca004d53f026e5dff
출처 데이터셋
uspto-grants-1991_01
특허 번호
US04985570

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