Nitric Acid → HCID 178433429, 화합물

HRID 1894637노트

반응식

HRID 1894637 반응식
[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

참가 물질

3

반응물 2

HCID 944Nitric AcidHCID 178423588HCID 178423588, 화합물

생성물 1

HCID 178433429HCID 178433429, 화합물

실험 절차

In a 500 ml single-necked round-bottomed flask, 230 ml of a 65% aqueous 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 aqueous 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.).

후처리

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

출처 및 근거

ORD 기록
ord-051c32b5d042483991b224eaae926b3e
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08513286B2

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