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

HRID 1600541노트

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HRID 1600541 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1e64df7a10724d769df6a59d43d01756
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05977027

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