Water → N-Acetyl-N-(3-ethoxycarbonylaminophenethyl)amine

HRID 1173127노트

반응식

HRID 1173127 반응식
[C:1]([NH:4][CH2:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([NH2:13])[CH:8]=1)(=[O:3])[CH3:2].Cl[C:15]([O:17][CH2:18][CH3:19])=[O:16].O>N1C=CC=CC=1>[C:1]([NH:4][CH2:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([NH:13][C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH:8]=1)(=[O:3])[CH3:2]

참가 물질

5

반응물 3

HCID 962WaterHCID 10928Ethyl chloroformateHCID 22674097N-Acetyl-N-(3-aminophenethyl)amine

생성물 1

HCID 22674171N-Acetyl-N-(3-ethoxycarbonylaminophenethyl)amine수율 97%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

N-Acetyl-N-(3-aminophenethyl)amine (1.7 g, Production Example 29b) was dissolved in pyridine (5 ml). Under ice-cooling, ethyl chloroformate (1.4 ml) was added dropwise thereinto, followed by stirring at room temperature for one hour. Then, the mixture was ice-cooled again and water was added thereto. The mixture was extracted with ethyl acetate, and the extract was washed with brine and dried over anhydrous magnesium sulfate. The solvent was evaporated, to give the title compound (2.358 g, 97%) as a yellow oil.

후처리

  1. temperatureUnder ice-cooling
  2. temperaturecooled again
  3. extractionThe mixture was extracted with ethyl acetate
  4. washthe extract was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-714c56258bdf47f3a5d4827d3a5d0379
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07834049B2

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