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

HRID 594107

反応式

HRID 594107 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-b3c093f525ae4ee4a14fadf76214e9a2
出典データセット
uspto-grants-2016_01
特許番号
US09242972B2

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