Ethyl 3-ethoxy-3-iminopropionate hydrochloride → 2,3,4-trifluoro-N-[1-ethoxy-2-(ethoxycarbonyl)ethylidene]aniline

HRID 344892

反応式

HRID 344892 の反応式
[F:1][C:2]1[C:8]([F:9])=[C:7]([F:10])[CH:6]=[CH:5][C:3]=1[NH2:4].Cl.[CH2:12]([O:14][C:15]([CH2:17][C:18](=N)[O:19][CH2:20][CH3:21])=[O:16])[CH3:13]>C(O)C>[F:1][C:2]1[C:8]([F:9])=[C:7]([F:10])[CH:6]=[CH:5][C:3]=1[N:4]=[C:18]([O:19][CH2:20][CH3:21])[CH2:17][C:15]([O:14][CH2:12][CH3:13])=[O:16]

参加物

4

反応物 2

HCID 75345Ethyl 3-ethoxy-3-iminopropionate hydrochlorideHCID 774682,3,4-Trifluoroaniline

生成物 1

HCID 186419482,3,4-trifluoro-N-[1-ethoxy-2-(ethoxycarbonyl)ethylidene]aniline収率 105.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
20 °C

実験手順

2,3,4-Trifluoroaniline (58.8 g) is added in a single portion with stirring to a solution of 2-ethoxycarbonyl-1-ethoxyethylideneamine hydrochloride (90 g) in ethanol (820 cc). After 48 hours' stirring at a temperature in the region of 20° C., the suspension obtained is filtered; the filtrate is concentrated under reduced pressure (20 kPa) at a temperature in the region of 50° C. The oily residue is taken up with water (250 cc). The mixture obtained is extracted with ethyl ether (3×200 cc). The combined organic extracts are washed with water (4×150 cc), dried over magnesium sulphate and concentrated under reduced pressure (20 kPa) at approximately 30° C. 2,3,4-Trifluoro-N-[1-ethoxy-2-(ethoxycarbonyl)ethylidene]aniline (122 g) is obtained in the form of a yellow oil, which is used without further purification for the subsequent steps.

後処理

  1. customthe suspension obtained
  2. filtrationis filtered
  3. concentrationthe filtrate is concentrated under reduced pressure (20 kPa) at a temperature in the region of 50° C
  4. customThe mixture obtained
  5. extractionis extracted with ethyl ether (3×200 cc)
  6. washThe combined organic extracts are washed with water (4×150 cc)
  7. dry with materialdried over magnesium sulphate
  8. concentrationconcentrated under reduced pressure (20 kPa) at approximately 30° C

出典と根拠

ORDレコード
ord-9c008d3139064a119e4be92090e7f59b
出典データセット
uspto-grants-1991_10
特許番号
US05053509

関連ノート

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