Barium nitrate → 1-Amino-3-bromo-4-methylpyridinium nitrate

HRID 1036143

反応式

HRID 1036143 の反応式
[O-2].[Ba+2].[N+:3]([O-:6])([O-:5])=[O:4].[Ba+2].[N+:8]([O-])([O-])=O.[Br:12][C:13]1[CH:14]=[N:15][CH:16]=[CH:17][C:18]=1[CH3:19]>O>[N+:3]([O-:6])([O-:5])=[O:4].[NH2:8][N+:15]1[CH:16]=[CH:17][C:18]([CH3:19])=[C:13]([Br:12])[CH:14]=1

参加物

5

反応物 3

HCID 24798Barium nitrateHCID 8176303-Bromo-4-methylpyridineHCID 9855530Barium Oxide Nanoparticle Dispersion

生成物 1

HCID 671269021-Amino-3-bromo-4-methylpyridinium nitrate収率 113.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

Barium oxide (950 mg, 90%, 5.56 mmol) were carefully added into 6 ml water in small portions followed by addition of barium nitrate (983 g, 3.76 mmol) and 3-bromo-4-methylpyridine (1.72 g, 10 mmol). The resulting suspension was stirred at r.t. and a solution of hydroxylamine O-sulfonic acid (995 mg, 8.36 mmol) in 2 ml water was added drop-wise. The white suspension was stirred at 90° C. for 15 h before cooling down to r.t. The white precipitate was filtered off and washed with water. The aqueous phase was evaporated to dryness to give 1.065 g of 205 as off-white solid (yield: 45.7%) which were directly used for next step without further purification.

後処理

  1. stirringThe white suspension was stirred at 90° C. for 15 h
  2. temperaturebefore cooling down to r.t
  3. filtrationThe white precipitate was filtered off
  4. washwashed with water
  5. customThe aqueous phase was evaporated to dryness

出典と根拠

ORDレコード
ord-2220ff6e706648f58ab047b57c6d6982
出典データセット
uspto-grants-2013_10
特許番号
US08546403B2

関連ノート

読み込み中…