Sodium Hydroxide → (4-Nitropyridin-2-yl)methanol

HRID 600263ノート

反応式

HRID 600263 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][N:7]=[C:6]([CH2:10][O:11]C(=O)C)[CH:5]=1)([O-:3])=[O:2].[OH-].[Na+]>CO>[N+:1]([C:4]1[CH:9]=[CH:8][N:7]=[C:6]([CH2:10][OH:11])[CH:5]=1)([O-:3])=[O:2]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 14761430(4-Nitropyridin-2-yl)methyl acetate

生成物 1

HCID 14761455(4-Nitropyridin-2-yl)methanol

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of acetic acid 4-nitro-pyridin-2-ylmethyl ester (16)(0.49 g, 2.5 mmol) in methanol (5 mL), was added a solution of sodium hydroxide (2N, 1.6 mL) and the reaction was stirred for 30 minutes and then concentrated in vacuo. The residue was diluted with water (10 mL) and extracted with ethyl acetate (2×10 mL). The combined extracts were washed with brine (10 mL) and concentrated in vacuo to afford a crude oil which solidified upon standing. Single peak in LC-MS analysis, (0.13 g 33%); m/z (LC-MS, ESP), RT=2.67 mins, (M+H) 155.

後処理

  1. concentrationconcentrated in vacuo
  2. additionThe residue was diluted with water (10 mL)
  3. extractionextracted with ethyl acetate (2×10 mL)
  4. washThe combined extracts were washed with brine (10 mL)
  5. concentrationconcentrated in vacuo
  6. customto afford a crude oil which

出典と根拠

ORDレコード
ord-5b7dff31fb944675a071fa21c386ddaf
出典データセット
uspto-grants-2011_03
特許番号
US07902193B2

反応ノート

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