Etofenprox → 3-Phenoxytoluene

HRID 2351806

Reaktionsgleichung

Reaktionsgleichung von HRID 2351806
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]([CH3:28])([CH3:27])[CH2:11][O:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([O:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH:15]=2)=[CH:6][CH:5]=1)[CH3:2].ClC1C=C(C(C)(C)COCC2C=CC=C(OC3C=CC=CC=3)C=2)C=CC=1OCC>C1C=CC=CC=1>[O:20]([C:16]1[CH:15]=[C:14]([CH3:13])[CH:19]=[CH:18][CH:17]=1)[C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1.[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]([CH3:27])([CH3:28])[CH2:11][OH:12])=[CH:6][CH:5]=1)[CH3:2]

Komponenten

5

Edukt 2

HCID 71245EtofenproxHCID 30671833-Chloro-4-ethoxyneophyl 3-phenoxybenzyl ether

Produkt 2

HCID 191653-PhenoxytolueneHCID 1585252-(4-Ethoxyphenyl)-2-methylpropanol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

The reaction mixture was cooled to 50° C. and the residual pressure was released, and 100 ml of benzene was added into the autoclave to dissolve the oil layer. Then, the catalyst was removed by filtration, and the filtrate was allowed to stand still to cause phase separation, and the benzene layer was recovered and washed with 120 ml of water three times, and benzene was removed by distillation under reduced pressure to give an oily product. From the results of the analysis of the oily product by gas chromatography according to the internal standard method, it was found that the oily product comprised 98.8% of 3-phenoxybenzyl 2-(4-ethoxyphenyl)-2-methylpropyl ether and 0.3% of unreacted starting 3-phenoxybenzyl 2-(3-chloro-4-ethoxyphenyl)-2-methylpropyl ether, and that the content of each of 3-phenoxytoluene and 4-ethoxyneophyl alcohol formed by cleaving of the ether linkage was lower than 0.3%. The amount of the obtained oily product was 53.8 g, and the yield was 96.7%.

Aufarbeitung

  1. dissolutionto dissolve the oil layer
  2. customThen, the catalyst was removed by filtration
  3. customphase separation
  4. customthe benzene layer was recovered
  5. washwashed with 120 ml of water three times, and benzene
  6. customwas removed by distillation under reduced pressure
  7. customto give an oily product
  8. customFrom the results of the analysis of the oily product by gas chromatography

Quellen und Nachweise

ORD-Eintrag
ord-413d38bb0cd042b7b6e224623631a215
Quelldatensatz
uspto-grants-1989_10
Patentnummer
US04873373

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