Sodium Carbonate → 2,2,6-Trimethylcyclohexyl 2-cyano-3,3-diphenylacrylate

HRID 2228360

反応式

HRID 2228360 の反応式
[C:1]([C:3](=[C:9]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[C:4](OCC)=[O:5])#[N:2].C([O-])([O-])=O.[Na+].[Na+].[CH3:28][C:29]1([CH3:37])[CH2:34][CH2:33][CH2:32][CH:31]([CH3:35])[CH:30]1[OH:36]>>[C:1]([C:3](=[C:9]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1)[C:4]([O:36][CH:30]1[CH:31]([CH3:35])[CH2:32][CH2:33][CH2:34][C:29]1([CH3:37])[CH3:28])=[O:5])#[N:2]

参加物

4

反応物 3

HCID 10340Sodium CarbonateHCID 243274EtocryleneHCID 125371292,2,6-Trimethylcyclohexan-1-ol

生成物 1

HCID 184696152,2,6-Trimethylcyclohexyl 2-cyano-3,3-diphenylacrylate収率 74%

実験手順

55.4 g (0.2 mol) of ethyl 2-cyano-3,3-diphenylacrylate (Uvinul 3035), 100 ml of 2,2,6-trimethylcyclohexanol and 4 g of Na2CO3 were reacted with one another at 184-186° C. with distillative removal of the ethanol formed, assisted by a stream of nitrogen. After about 3 h, the reaction mixture was filtered hot in order to remove the Na2CO3. After the filtrate had been cooled, it was distilled under reduced pressure, giving 55 g (74%) of 2,2,6-trimethylcyclohexyl 2-cyano-3,3-diphenylacrylate [λmax=304 nm, E11=351] as a colorless solid.

後処理

  1. customwith distillative removal of the ethanol
  2. customformed
  3. filtrationthe reaction mixture was filtered hot in order
  4. customto remove the Na2CO3
  5. temperatureAfter the filtrate had been cooled
  6. distillationit was distilled under reduced pressure

出典と根拠

ORDレコード
ord-883c05c243f44e6ababfff6e592502a2
出典データセット
uspto-grants-2002_07
特許番号
US06416773B2

関連ノート

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