Acetone → 1,3-Bis-(4-benzoyl-3-hydroxyphenoxy)-prop-2-yl 2-cyano-3,3-dimethylacrylate

HRID 621664

反応式

HRID 621664 の反応式
FC(F)(F)S(O)(=O)=O.[C:9]([CH2:11][C:12]([O:14][CH:15]([CH2:33][O:34][C:35]1[CH:40]=[CH:39][C:38]([C:41](=[O:48])[C:42]2[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=2)=[C:37]([OH:49])[CH:36]=1)[CH2:16][O:17][C:18]1[CH:23]=[CH:22][C:21]([C:24](=[O:31])[C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[C:20]([OH:32])[CH:19]=1)=[O:13])#[N:10].[CH3:50][C:51]([CH3:53])=O>>[C:9]([C:11](=[C:51]([CH3:53])[CH3:50])[C:12]([O:14][CH:15]([CH2:16][O:17][C:18]1[CH:23]=[CH:22][C:21]([C:24](=[O:31])[C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)=[C:20]([OH:32])[CH:19]=1)[CH2:33][O:34][C:35]1[CH:40]=[CH:39][C:38]([C:41](=[O:48])[C:42]2[CH:43]=[CH:44][CH:45]=[CH:46][CH:47]=2)=[C:37]([OH:49])[CH:36]=1)=[O:13])#[N:10]

参加物

4

反応物 3

HCID 180AcetoneHCID 62406Trifluoromethanesulfonic acidHCID 538270821,3-Bis-(4-benzoyl-3-hydroxyphenoxy)-prop-2-yl cyanoacetate

生成物 1

HCID 543990671,3-Bis-(4-benzoyl-3-hydroxyphenoxy)-prop-2-yl 2-cyano-3,3-dimethylacrylate収率 86%

反応条件

温度
56 °C

実験手順

1 g of trifluoromethanesulfonic acid was added to a solution of 55.2 g (0.1 mole) of 1,3-bis-(4-benzoyl-3-hydroxyphenoxy)-prop-2-yl cyanoacetate in 300 ml of acetone, and the solution was heated for 3 hours at a temperature of 56° C. After cooling to room temperature, the resulting crystalline precipitate was filtered off with suction and recrystallized from acetone. After drying, 51 g (86 percent of theory) of 1,3-bis-(4-benzoyl-3-hydroxyphenoxy)-prop-2-yl 2-cyano-3,3-dimethylacrylate were obtained in the form of colorless crystals having a melting point of 145° to 147° C. and a purity of 99 percent (HPLC). The structure of the compound obtained was confirmed by UV, IR and NMR spectra.

後処理

  1. temperatureAfter cooling to room temperature
  2. filtrationthe resulting crystalline precipitate was filtered off with suction
  3. customrecrystallized from acetone
  4. customAfter drying

出典と根拠

ORDレコード
ord-d1be10188bd749ccb265edf5ad1c132b
出典データセット
uspto-grants-1989_04
特許番号
US04824892

関連ノート

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