Nitric Acid → HCID 178433429、化合物

HRID 508461ノート

反応式

HRID 508461 の反応式
[N+:1]([O-:4])(O)=[O:2].[Br:5][C:6]1[C:7]([OH:13])=[N:8][C:9]([CH3:12])=[CH:10][CH:11]=1>>[Br:5][C:6]1[C:7]([OH:13])=[N:8][C:9]([CH3:12])=[C:10]([N+:1]([O-:4])=[O:2])[CH:11]=1

参加物

3

反応物 2

HCID 944Nitric AcidHCID 178423588HCID 178423588、化合物

生成物 1

HCID 178433429HCID 178433429、化合物

実験手順

In a 500 ml single-necked round-bottomed flask, 230 ml of a 65% ageous HNO3 solution is added and stirred under cooling (ice/water cooling bath). 7.00 g of 3-bromo-6-methyl-pyridin-2-ol 2 at ambient temperature is introduced portion-wise. Stirring is continued for 3.5 hours at ambient temperature. After pouring the mixture into 200 ml of an ice/water mixture (pH 1), the water phase is extracted with AcOEt. The organic phase is washed twice with water brought to pH 4 by adding ageous NaOH solution (pH meter), then dried over sodium sulfate, filtered and concentrated in vacuo to give 7.52 g of a yellow solid. This crude material is suspended in diethyl ether and stirred for 1 hour at ambient temperature, filtered, washed with the same solvent and dried to give 3.89 g of the compound as a yellow-orange solid (m.p. >220° C.).

後処理

  1. stirringStirring
  2. extractionthe water phase is extracted with AcOEt
  3. washThe organic phase is washed twice with water
  4. additionby adding ageous NaOH solution (pH meter)
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-e7f5a5985c9944e88e8068f7a9b512b7
出典データセット
uspto-grants-2015_08
特許番号
US09096525B2

反応ノート

読み込み中…