Sodium Carbonate → HCID 178422452、化合物

HRID 1366174ノート

反応式

HRID 1366174 の反応式
[CH3:1][C:2]1[N:7]=[C:6]([OH:8])[CH:5]=[C:4](O)[CH:3]=1.P(Br)(Br)([Br:12])=O.C([O-])([O-])=O.[Na+].[Na+]>CN(C=O)C.O>[Br:12][C:4]1[CH:3]=[C:2]([CH3:1])[N:7]=[C:6]([OH:8])[CH:5]=1

参加物

6

反応物 3

HCID 10340Sodium CarbonateHCID 24613Phosphorus oxybromideHCID 178429093HCID 178429093、化合物

生成物 1

HCID 178422452HCID 178422452、化合物収率 46.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
110 °C

実験手順

A solution of 6-methylpyridine-2,4-diol (1.75 g, 14.0 mmol) in dry DMF (6.0 mL) is stirred under N2 and phosphorus oxybromide (3.05 g, 10.6 mmol) is added in one portion. The mixture is heated at 110° C. for 45 min and then cooled and diluted with water (7 mL). Na2CO3 (s) is added to bring the pH to 7 and the resulting suspension is cooled to 0° C. The product is collected by suction filtration, rinsing with cold water and diethyl ether, and dried overnight in a vacuum desiccator to afford the title compound as a light brown solid (920 mg).

後処理

  1. temperaturecooled
  2. temperaturethe resulting suspension is cooled to 0° C
  3. filtrationThe product is collected by suction filtration
  4. washrinsing with cold water and diethyl ether
  5. customdried overnight in a vacuum desiccator

出典と根拠

ORDレコード
ord-bb6e4080a9ce4aa08e6d437351247d47
出典データセット
uspto-grants-2011_02
特許番号
US07893058B2

反応ノート

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