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

HRID 704090

反応式

HRID 704090 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 176Acetic Acid溶媒2 回

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3586a230fbe5452ca004d53f026e5dff
出典データセット
uspto-grants-1991_01
特許番号
US04985570

関連ノート

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