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Phenol → HCID 19979676、化合物

HRID 1461889
ノート
印刷プレビュー

反応式

HRID 1461889 の反応式
[C:1]([C:5]1[CH:6]=[C:7]([CH2:12][CH2:13][C:14]([OH:16])=[O:15])[CH:8]=[CH:9][C:10]=1[OH:11])([CH3:4])([CH3:3])[CH3:2].[C:17]1(O)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.CN(C)C=O.P(Cl)(Cl)(Cl)=O>C1(C)C=CC=CC=1>[C:1]([C:5]1[CH:6]=[C:7]([CH2:12][CH2:13][C:14]([O:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[O:15])[CH:8]=[CH:9][C:10]=1[OH:11])([CH3:4])([CH3:2])[CH3:3]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 996PhenolHCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 54637793-(3-tert-Butyl-4-hydroxyphenyl)propanoic acid

生成物 1

HCID 19979676HCID 19979676、化合物収率 90.1%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
70 °C

実験手順

A mixture of 55 g of 3-(3-tert-butyl-4-hydroxyphenyl)-propionic acid, 35 g of phenol, 7 g of dimethylformamide, 19.1 g of phosphorus oxychloride and 250 ml of toluene was stirred at 70° C. for 6 hours. The mixture was cooled to room temperature, and 800 ml of toluene was added thereto. The mixture was washed with water and an aqueous solution of sodium hydroxide, followed by washing with water. The mixture was concentrated, and the residue was purified by silica gel column chromatography to give 66.5 g of phenyl 3-(3-tert-butyl-4-hydroxyphenyl)propionate as a white crystal, m.p. 106°-109° C.

後処理

  1. temperatureThe mixture was cooled to room temperature
  2. washThe mixture was washed with water
  3. washby washing with water
  4. concentrationThe mixture was concentrated
  5. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-319b8e45869d424aae9fc361fef4f873
出典データセット
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05077424

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート