Dichloromethane → (Z)-3-(3-nitro-4-methoxyphenyl)-2-(3,4,5-trimethoxyphenyl)-prop-2-ene-nitrile

HRID 260096

反応式

HRID 260096 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][C:11]=1[O:12][CH3:13])[CH:7]=O)([O-:3])=[O:2].[CH3:14][O:15][C:16]1[CH:17]=[C:18]([CH2:26][C:27]#[N:28])[CH:19]=[C:20]([O:24][CH3:25])[C:21]=1[O:22][CH3:23].[OH-].[Na+].ClCCl>O.[Cl-].C([NH2+]C)CCCCCCC>[N+:1]([C:4]1[CH:5]=[C:6](/[CH:7]=[C:26](/[C:18]2[CH:19]=[C:20]([O:24][CH3:25])[C:21]([O:22][CH3:23])=[C:16]([O:15][CH3:14])[CH:17]=2)\[C:27]#[N:28])[CH:9]=[CH:10][C:11]=1[O:12][CH3:13])([O-:3])=[O:2]

参加物

7

反応物 4

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 258873,4,5-TrimethoxyphenylacetonitrileHCID 7006084-Methoxy-3-nitrobenzaldehyde

生成物 1

HCID 10619131(Z)-3-(3-nitro-4-methoxyphenyl)-2-(3,4,5-trimethoxyphenyl)-prop-2-ene-nitrile収率 72.4%

試薬・触媒・溶媒 2

HCID 22561414HCID 22561414、化合物触媒HCID 962Water溶媒

実験手順

3.0 g of 3-nitro-4-methoxybenzaldehyde, 3.4 g of 3,4,5-trimethoxyphenylacetonitrile, 800 mg of sodium hydroxide and 100 mg of octylmethylammonium chloride were dissolved in 15 ml of water and 15 ml of dichloromethane and reacted for 4 hours at room temperature. Ice water was added to the reaction liquid, which was then extracted three times each with dichloromethane. The extract was dried with anhydrous sodium sulfate and concentrated. The concentrated liquid was purified by crystallization (ethyl acetate) to obtain 4.4 g of the intended compound. The yield was 72%.

後処理

  1. extractionwas then extracted three times each with dichloromethane
  2. dry with materialThe extract was dried with anhydrous sodium sulfate
  3. concentrationconcentrated
  4. customThe concentrated liquid was purified by crystallization (ethyl acetate)

出典と根拠

ORDレコード
ord-1fc0a5e64cea4a7692a615b3c55a2b09
出典データセット
uspto-grants-1996_06
特許番号
US05525632

関連ノート

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