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Sodium Hydroxide → HCID 23614955, 화합물

HRID 1985996
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HRID 1985996 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

HCID 23614955HCID 23614955, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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-acetoxystyrene) 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.

후처리

  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

출처 및 근거

ORD 기록
ord-09ed6479c6134e6b984b16a70719f50b
출처 데이터셋
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07547749B2

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