2,6-Dimethylphenol → Bis(2,6-dimethylphenyl) Chlorophosphate

HRID 2367919ノート

反応式

HRID 2367919 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[OH:9].[Cl-].[Mg+2].[Cl-].[P:13]([Cl:17])(Cl)(Cl)=[O:14]>O>[C:3]1([O:9][P:13]([Cl:17])(=[O:14])[O:9][C:3]2[C:4]([CH3:8])=[CH:5][CH:6]=[CH:7][C:2]=2[CH3:1])[C:4]([CH3:8])=[CH:5][CH:6]=[CH:7][C:2]=1[CH3:1]

参加物

5

反応物 3

HCID 113352,6-DimethylphenolHCID 24813Phosphorus oxychlorideHCID 5360315Magnesium Chloride

生成物 1

HCID 9923313Bis(2,6-dimethylphenyl) Chlorophosphate

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
120 °C

実験手順

A 1,000-ml four-necked flask provided with a stirring machine, a temperature gauge, a dropping funnel, and a nitrogen-introducing pipe was mounted with a condenser to which a water scrubber had been connected, and then 2.0 mol (244 g) of 2,6-dimethylphenol, and 0.016 mol (1.5 g) of magnesium chloride were loaded into the resultant reactor. The atmosphere in the reactor was replaced with nitrogen and then its temperature was increased to 120° C. 1.0 Mole (153 g) of phosphorus oxychloride was dropped to the reactor at the temperature over 2 hours. After the completion of the dropping, the temperature was increased to 180° C. over 2 hours. Thus, di(2,6-xylyl)phosphorochloridate was obtained. The temperature in the flask was cooled to 20° C., and then 0.5 mol (55 g) of 1,3-benzenediol and 0.016 mol (1.5 g) of magnesium chloride were loaded into the flask. The temperature was increased to 180° C. over 2 hours and then the mixture was aged for 2 hours. After that, the catalyst was removed by an ordinary method and then the remainder was dried at 140° C. under reduced pressure. Thus, B-3 represented by general formula (24) was obtained.

後処理

  1. customA 1,000-ml four-necked flask provided with a stirring machine
  2. additiona temperature gauge, a dropping funnel, and a nitrogen-introducing pipe
  3. customwas mounted with a condenser to which
  4. temperatureAfter the completion of the dropping, the temperature was increased to 180° C. over 2 hours

出典と根拠

ORDレコード
ord-76c313338bb3449fb0a9e04a6c5170db
出典データセット
uspto-grants-2014_04
特許番号
US08703674B2

反応ノート

読み込み中…