Water → HCID 54408223、化合物

HRID 277294

反応式

HRID 277294 の反応式
[C:1]([C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH:6]=[O:7])#[N:2].[CH3:11][C:12]([C:14]1[CH:19]=[C:18]([C:20]#[N:21])[CH:17]=[CH:16][CH:15]=1)=O.OS(O)(=O)=O.O>C(O)(=O)C>[C:20]([C:18]1[CH:19]=[C:14]([CH:12]=[CH:11][C:6]([C:5]2[CH:8]=[CH:9][CH:10]=[C:3]([C:1]#[N:2])[CH:4]=2)=[O:7])[CH:15]=[CH:16][CH:17]=1)#[N:21]

参加物

6

反応物 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 802223-AcetylbenzonitrileHCID 90670m-Formylbenzonitrile

生成物 1

HCID 54408223HCID 54408223、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

3-Cyanobenzaldehyde (3.0 g, 23.0 mmol) and 3-cyanoacetophenone (3.34 g, 23.0 mmol) in glacial acetic acid (5 mL) and concentrated H2SO4 (3.66 mL, 69 mmol) was stirred at room temperature for 72 hours. Water (200 mL) was added and the reaction filtered. The precipitate was washed with water (2×200 mL) and dried in vacuo to give 3,3′-dicyanochalcone as an off-white solid. MS (APCI) m/z 258 (M+−1, 100%). 13C NMR (50 MHz, d6-DMSO): δ111.7, 117.8, 118.0, 123.0, 129.7, 131.6, 132.1, 132.4, 133.3, 133.5, 135.3, 136.1, 137.4, 142.1, 187.3.

後処理

  1. filtrationthe reaction filtered
  2. washThe precipitate was washed with water (2×200 mL)
  3. customdried in vacuo

出典と根拠

ORDレコード
ord-14ffe8cfbb58484792efb5d5d57e1733
出典データセット
uspto-grants-2002_03
特許番号
US06355683B1

関連ノート

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