Sodium Chloride → (Z)-1,2,3-trimethoxy-5-(4-methoxy-3-nitrostyryl)benzene

HRID 260091

반응식

HRID 260091 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].[Br-].[CH3:15][O:16][C:17]1[CH:18]=[C:19]([CH:40]=[C:41]([O:45][CH3:46])[C:42]=1[O:43][CH3:44])[CH2:20]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:20]\[C:19]2[CH:40]=[C:41]([O:45][CH3:46])[C:42]([O:43][CH3:44])=[C:17]([O:16][CH3:15])[CH:18]=2)[CH:9]=[CH:10][C:11]=1[O:12][CH3:13])([O-:3])=[O:2]

참가 물질

7

반응물 4

HCID 5234Sodium ChlorideHCID 24758Sodium hydrideHCID 7006084-Methoxy-3-nitrobenzaldehydeHCID 178418302HCID 178418302, 화합물

생성물 1

HCID 10617491(Z)-1,2,3-trimethoxy-5-(4-methoxy-3-nitrostyryl)benzene수율 43.3%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 241Benzene용매2회

실험 절차

1.54 g of 3-nitro-4-methoxybenzaldehyde and 4.45 g of 3,4,5-trimethoxybenzyltriphenylphosphine bromide were dissolved in 40 ml of benzene, and a benzene solution containing 408 mg of sodium hydride dispersed therein was added thereto and reacted for 15 hours at room temperature (about 20°-30° C.). The reaction mixture 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 (ethyl acetate:hexane=1:2 by volume) to obtain 1.27 g of the intended compound. The yield of the product was 43%.

후처리

  1. additiondispersed
  2. additiontherein was added
  3. customreacted for 15 hours at room temperature (about 20°-30° C.)
  4. additionwas added
  5. extractionthe resulting liquid was extracted with dichloromethane
  6. dry with materialThe extract was dried with anhydrous sodium sulfate
  7. concentrationconcentrated
  8. custompurified by silica gel column chromatography (ethyl acetate:hexane=1:2 by volume)

출처 및 근거

ORD 기록
ord-e7bc58f006fb4be784d38370b9d81678
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05525632

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