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

HRID 260096

반응식

HRID 260096 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 22561414HCID 22561414, 화합물촉매HCID 962Water용매

실험 절차

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%.

후처리

  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)

출처 및 근거

ORD 기록
ord-1fc0a5e64cea4a7692a615b3c55a2b09
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05525632

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