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Hydrochloric Acid → HCID 53917946, 화합물

HRID 1359576
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HRID 1359576 반응식
[N+:1]([C:4]1[CH:21]=[CH:20][C:7]([C:8]([C:10]2[CH:17]=[C:16]([O:18][CH3:19])[CH:15]=[CH:14][C:11]=2[CH:12]=O)=[O:9])=[CH:6][CH:5]=1)([O-:3])=[O:2].[Cl-].[CH3:23][O:24][CH2:25][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.O.Cl>C1(C)C=CC=CC=1>[CH3:23][O:24][CH:25]=[CH:12][C:11]1[CH:14]=[CH:15][C:16]([O:18][CH3:19])=[CH:17][C:10]=1[C:8](=[O:9])[C:7]1[CH:20]=[CH:21][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 2723798Methoxymethyl-triphenylphosphonium chlorideHCID 158394314-Methoxy-2-(4-nitrobenzoyl)benzaldehyde

생성물 1

HCID 53917946HCID 53917946, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

10 g of 2-(4-nitrobenzoyl)-4-methoxybenzaldehyde is introduced together with 18 g of (methoxymethyl)triphenylphosphonium chloride in 400 ml of toluene and mixed in portions with 5.9 g of potassium-tert-butylate while being cooled with ice. After 1 hour of stirring while being cooled with ice and a subsequent 3.5 hours of stirring at room temperature, it is mixed with 200 ml of water, weakly acidified with 1N hydrochloric acid and extracted three times with ethyl acetate. The ethyl acetate phases are washed with saturated common salt solution, dried, filtered and concentrated by evaporation. The residue is chromatographed on silica gel with hexane:ethyl acetate=1:1 as an eluant. 6.9 g of 1-methoxy-2-(4-methoxy-2-(4-nitrobenzoyl)phenyl)ethylene as a mixture of the E- and Z-forms is obtained.

후처리

  1. temperaturewhile being cooled with ice
  2. temperaturewhile being cooled with ice and a subsequent 3.5 hours
  3. stirringof stirring at room temperature
  4. extractionextracted three times with ethyl acetate
  5. washThe ethyl acetate phases are washed with saturated common salt solution
  6. customdried
  7. filtrationfiltered
  8. concentrationconcentrated by evaporation
  9. customThe residue is chromatographed on silica gel with hexane
  10. addition6.9 g of 1-methoxy-2-(4-methoxy-2-(4-nitrobenzoyl)phenyl)ethylene as a mixture of the E-
  11. customZ-forms is obtained

출처 및 근거

ORD 기록
ord-1e8977e6ba59437695fefce1813347d8
출처 데이터셋
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06600036B2

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