Ethanolamine → Methyl 2-[(2-hydroxyethyl)amino]-3-nitrobenzoate

HRID 1698537노트

반응식

HRID 1698537 반응식
Cl[C:2]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].[CH2:15]([NH2:18])[CH2:16][OH:17]>C1COCC1>[OH:17][CH2:16][CH2:15][NH:18][C:2]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5]

참가 물질

4

반응물 2

HCID 700EthanolamineHCID 10751184Methyl 2-chloro-3-nitrobenzoate

생성물 1

HCID 11253443Methyl 2-[(2-hydroxyethyl)amino]-3-nitrobenzoate수율 95%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 4.70 g (21.9 mmol) of methyl 2-chloro-3-nitrobenzoate in 300 mL of THF was added dropwise 300 mL of 2-ethanolamine (80 mmol) and the mixture was refluxed over night. The reaction was concentrated to dryness, dissolved in ethyl acetate, and washed aqueous sodium hydrogen carbonate and water. The organics were dried over magnesium sulfate, filtered, and concentrated in vacuo to give 5.00 g (20.8 mmol, 95%) of the title compound.

후처리

  1. temperaturethe mixture was refluxed over night
  2. concentrationThe reaction was concentrated to dryness
  3. dissolutiondissolved in ethyl acetate
  4. washwashed aqueous sodium hydrogen carbonate and water
  5. dry with materialThe organics were dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-2f13086cd1804c98ba47649a0c989326
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08163935B2

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