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

HRID 1173127ノート

反応式

HRID 1173127 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 22674171N-Acetyl-N-(3-ethoxycarbonylaminophenethyl)amine収率 97%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-714c56258bdf47f3a5d4827d3a5d0379
出典データセット
uspto-grants-2010_11
特許番号
US07834049B2

反応ノート

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