Methyl Chloride → 6-(2,4-Dimethoxybenzoyl)-(6H)-dibenz[c,e][1,2]-oxaphosphorin 6-oxide

HRID 1085366

Reaktionsgleichung

Reaktionsgleichung von HRID 1085366
[CH3:1][O:2][C:3]1[CH:11]=[C:10]([O:12][CH3:13])[CH:9]=[CH:8][C:4]=1[C:5](Cl)=[O:6].C[O:15][P:16]1[C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=2[C:19]2[CH:26]=[CH:27][CH:28]=[CH:29][C:18]=2[O:17]1.CCl>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:11]=[C:10]([O:12][CH3:13])[CH:9]=[CH:8][C:4]=1[C:5]([P:16]1(=[O:15])[C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=2[C:19]2[CH:26]=[CH:27][CH:28]=[CH:29][C:18]=2[O:17]1)=[O:6]

Komponenten

5

Edukt 3

HCID 6327Methyl ChlorideHCID 27347192,4-Dimethoxybenzoyl chlorideHCID 114361486-methoxy-(6H)-dibenz[c,e][1,2]-oxaphosphorin

Produkt 1

HCID 143662886-(2,4-Dimethoxybenzoyl)-(6H)-dibenz[c,e][1,2]-oxaphosphorin 6-oxide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

35.1 g (0.175 mol) of 2,4-dimethoxybenzoyl chloride were warmed to 70° C. under a nitrogen atmosphere. 40.3 g (0.175 mol) of 6-methoxy-(6H)-dibenz[c,e][1,2]oxaphosphorin were added dropwise in the course of two hours while stirring. The temperature was then slowly increased to 110° C. It was kept at this temperature until evolution of methyl chloride could no longer be detected. After cooling to 60° C., 70 ml of toluene were added. After crystallization, 50 g (75% of theory) of the abovementioned compound of melting point 112° to 115° C. were obtained.

Aufarbeitung

  1. temperatureAfter cooling to 60° C.
  2. customAfter crystallization, 50 g (75% of theory) of the abovementioned compound of melting point 112° to 115° C.
  3. customwere obtained

Quellen und Nachweise

ORD-Eintrag
ord-59980c4490ac4bf896a9b90d2f1be2cb
Quelldatensatz
uspto-grants-1991_04
Patentnummer
US05008426

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