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Sodium Hydroxide → HCID 23614955、化合物

HRID 1768159
ノート
印刷プレビュー

反応式

HRID 1768159 の反応式
Cl[C:2]1[N:7]=[C:6]([Cl:8])[N:5]=[C:4]([O:9][C:10]2[C:15]([CH3:16])=[CH:14][C:13]([CH3:17])=[CH:12][C:11]=2[CH3:18])[N:3]=1.[OH:19][C:20]1[CH:27]=[CH:26][C:23]([CH:24]=[CH2:25])=[CH:22][CH:21]=1.[OH-].[Na+]>ClCCl>[Cl:8][C:6]1[N:7]=[C:2]([O:19][C:20]2[CH:27]=[CH:26][C:23]([CH:24]=[CH2:25])=[CH:22][CH:21]=2)[N:3]=[C:4]([O:9][C:10]2[C:15]([CH3:16])=[CH:14][C:13]([CH3:17])=[CH:12][C:11]=2[CH3:18])[N:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 624534-VinylphenolHCID 110980692,4-Dichloro-6-(2,4,6-trimethylphenoxy)-1,3,5-triazine

生成物 1

HCID 23614955HCID 23614955、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 25.57 g (0.09 moles) 2,4-dichloro-6-(2,4,6-trimethylphenoxy)-1,3,5-triazine in 300 ml of dichloromethane was treated with 11.8 g (0.098 moles) p-hydroxystyrene (prepared by hydrolysis of p-acetoxystyiene) dissolved in about 40 ml dichloromethane. The mixture was cooled in an ice-water bath and 36.8 g of 10% aqueous sodium hydroxide solution was added with stirring over about 5 minutes. Stirring was continued for 30 minutes after which time the ice-water bath was removed and stirring was continued for about 2 hours. The mixture was treated with brine, the layers were separated, and after standing, the organic layer was washed twice with brine, and once with water, and dried over magnesium sulfate. Filtration and evaporation gave a white solid with proton NMR spectrum consistent with the desired product, 2-chloro-4-(4-ethenylphenoxy)-6-(2,4,6-trimethylphenoxy)-1,3,5-triazine.

後処理

  1. temperatureThe mixture was cooled in an ice-water bath
  2. stirringStirring
  3. waitwas continued for 30 minutes
  4. customafter which time the ice-water bath was removed
  5. stirringstirring
  6. waitwas continued for about 2 hours
  7. additionThe mixture was treated with brine
  8. customthe layers were separated
  9. washthe organic layer was washed twice with brine
  10. dry with materialonce with water, and dried over magnesium sulfate
  11. filtrationFiltration and evaporation

出典と根拠

ORDレコード
ord-77aabdd2fc8b41d2b82ec82570259fc3
出典データセット
uspto-grants-2007_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07235611B2

反応ノート

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