Water → Ethyl 2-[3-phenyl-1-(3-chloropropyl)ureido]isobutyrate

HRID 1600541ノート

反応式

HRID 1600541 の反応式
[C:1]1([N:7]=[C:8]=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl:10][CH2:11][CH2:12][CH2:13][NH:14][C:15]([CH3:22])([CH3:21])[C:16]([O:18][CH2:19][CH3:20])=[O:17].O>C1(C)C=CC=CC=1>[C:1]1([NH:7][C:8](=[O:9])[N:14]([C:15]([CH3:21])([CH3:22])[C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH2:13][CH2:12][CH2:11][Cl:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 962WaterHCID 7672Phenyl isocyanateHCID 21829920Ethyl 2-(3-chloropropylamino)isobutyrate

生成物 1

HCID 21829914Ethyl 2-[3-phenyl-1-(3-chloropropyl)ureido]isobutyrate収率 96.3%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
0 °C

実験手順

Phenyl isocyanate (2.8 g) was added to a solution of the above crude ethyl 2-(3-chloropropylamino)isobutyrate (5 g) in toluene (30 mL) which was cooled to 0° C., and the mixture was stirred overnight at 0° C. to room temperature. After adding water, the reaction solution was extracted with ethyl acetate. The organic layer was washed with water, dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure to give 7.4 g of crude ethyl 2-[3-phenyl-1-(3-chloropropyl)ureido]isobutyrate.

後処理

  1. extractionthe reaction solution was extracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-1e64df7a10724d769df6a59d43d01756
出典データセット
uspto-grants-1999_11
特許番号
US05977027

反応ノート

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