Ethanolamine → 2-((6-Methyl-5-nitropyridin-2-yl)amino)ethanol

HRID 594107노트

반응식

HRID 594107 반응식
Br[C:2]1[N:7]=[C:6]([CH3:8])[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][CH:3]=1.[CH2:12]([CH2:14][NH2:15])[OH:13]>C(O)C>[CH3:8][C:6]1[N:7]=[C:2]([NH:15][CH2:14][CH2:12][OH:13])[CH:3]=[CH:4][C:5]=1[N+:9]([O-:11])=[O:10]

참가 물질

4

반응물 2

HCID 700EthanolamineHCID 247280146-Bromo-2-methyl-3-nitropyridine

생성물 1

HCID 112178252-((6-Methyl-5-nitropyridin-2-yl)amino)ethanol수율 92.4%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

6-bromo-2-methyl-3-nitropyridine (2 g, 9.22 mmol) was dissolved in ethanol (20 mL) and to this solution was added ethanolamine (1.115 mL, 18.43 mmol). The reaction was left to stir overnight under nitrogen, at room temperature. The reaction was concentrated in vacuo, then diluted with ethyl acetate and saturated sodium bicarbonate solution. The organic phase was separated and washed with saturated sodium bicarbonate and brine, then dried using a hydrophobic frit and concentrated in vacuo to give the title compound as a yellow solid (1.68 g). Crude material used directly in next step, without further purification. LCMS (2 min, formic) Rt 0.60 min, m/z (ES+) 198 (M+H).

후처리

  1. waitThe reaction was left
  2. concentrationThe reaction was concentrated in vacuo
  3. additiondiluted with ethyl acetate and saturated sodium bicarbonate solution
  4. customThe organic phase was separated
  5. washwashed with saturated sodium bicarbonate and brine
  6. customdried
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-b3c093f525ae4ee4a14fadf76214e9a2
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09242972B2

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