Sodium Carbonate → Norbornyl 2-cyano-3,3-diphenylacrylate

HRID 2228359

反応式

HRID 2228359 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]([O:6][CH2:7][CH3:8])=[O:5])#[N:2].[CH2:22]1C2C[CH:28](O)[CH:24]([CH2:25]2)[CH2:23]1.C([O-])([O-])=O.[Na+].[Na+]>>[C:1]([C:3](=[C:9]([C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1)[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1)[C:4]([O:6][C:7]12[CH2:28][CH:24]([CH2:23][CH2:22]1)[CH2:25][CH2:8]2)=[O:5])#[N:2]

参加物

4

反応物 3

HCID 10340Sodium CarbonateHCID 790282-NorbornanolHCID 243274Etocrylene

生成物 1

HCID 70187991Norbornyl 2-cyano-3,3-diphenylacrylate収率 53.9%

実験手順

55.4 g (0.2 mol) of ethyl 2-cyano-3,3-diphenylacrylate (Uvinul 3035), 100 g of norborneol and 4 g of Na2CO3 were reacted with one another at about 185° C. with distillative removal of the ethanol formed, assisted by a stream of nitrogen. After about 4 h, the reaction mixture was filtered hot in order to remove the Na2CO3. After the filtrate had been cooled, the precipitate which had formed was filtered off, washed with cyclohexane and dried, giving 37 g (53%) of norbornyl 2-cyano-3,3-diphenylacrylate [λmax=304 nm, E11 =386] 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. customthe precipitate which had formed
  7. filtrationwas filtered off
  8. washwashed with cyclohexane
  9. customdried

出典と根拠

ORDレコード
ord-ab43598590c242b88933dd35a5902db4
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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