Sodium Chloride → (Z)-1-(3-nitro-4-chlorophenyl)-2-(3,4,5-trimethoxyphenyl)ethene

HRID 2897

反応式

HRID 2897 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][C:11]=1[Cl:12])[CH:7]=O)([O-:3])=[O:2].[Br-].[CH3:14][O:15][C:16]1[CH:17]=[C:18]([CH:39]=[C:40]([O:44][CH3:45])[C:41]=1[O:42][CH3:43])[CH2:19]P(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[H-].[Na+].[Cl-].[Na+]>C1C=CC=CC=1.C(O)(=O)C>[N+:1]([C:4]1[CH:5]=[C:6](/[CH:7]=[CH:19]\[C:18]2[CH:39]=[C:40]([O:44][CH3:45])[C:41]([O:42][CH3:43])=[C:16]([O:15][CH3:14])[CH:17]=2)[CH:9]=[CH:10][C:11]=1[Cl:12])([O-:3])=[O:2]

参加物

7

反応物 4

HCID 5234Sodium ChlorideHCID 24758Sodium hydrideHCID 855054-Chloro-3-nitrobenzaldehydeHCID 178418302HCID 178418302、化合物

生成物 1

HCID 10760270(Z)-1-(3-nitro-4-chlorophenyl)-2-(3,4,5-trimethoxyphenyl)ethene収率 50.9%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 241Benzene溶媒2 回

実験手順

1.0 g of 3-nitro-4-chlorobenzaldehyde and 2.8 g of 3,4,5-trimethoxybenzyltriphenylphosphine bromide were dissolved in 50 ml of benzene, and a benzene solution containing 260 mg of sodium hydride dispersed therein was added thereto and reacted for 15 hours at room temperature. The reaction liquid was neutralized with acetic acid, saturated sodium chloride solution was added thereto, and the resulting liquid was extracted with dichloromethane. The extract was dried with anhydrous sodium sulfate, concentrated and then purified by silica gel column chromatography diethyl (ether:hexane--1:2 by volume) to obtain 0.95 g of the intended compound. The yield of the product was 50.4%.

後処理

  1. additiondispersed
  2. additiontherein was added
  3. customreacted for 15 hours at room temperature
  4. customThe reaction liquid
  5. additionwas added
  6. extractionthe resulting liquid was extracted with dichloromethane
  7. dry with materialThe extract was dried with anhydrous sodium sulfate
  8. concentrationconcentrated
  9. custompurified by silica gel column chromatography diethyl (ether:hexane--1:2 by volume)

出典と根拠

ORDレコード
ord-7682e2cee87a4592adfa5b6aefdb5c2b
出典データセット
uspto-grants-1998_03
特許番号
US05731353

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