2-(2-Hydroxyphenyl)phenylphosphonic acid → CID 37314

HRID 1596698

Reaktionsgleichung

O[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[P:14](=[O:17])([OH:16])O>O1CCCC1>[CH:10]1[C:9]2[PH:14](=[O:16])[O:17][C:2]3[C:3](=[CH:4][CH:5]=[CH:6][CH:7]=3)[C:8]=2[CH:13]=[CH:12][CH:11]=1

Komponenten

Reaktionsbedingungen

Temperatur: 106 °C

Versuchsvorschrift

500 g of 2-(2-hydroxyphenyl)phenylphosphonic acid (HPPA) was placed in a 300 ml flask which was connected to a vacuum system. The content was heated to its molten state (106° C.) under full vacuum for dehydration. The temperature was slowly increased from 106 to 160° C. until the dehydration was complete. White solids of DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) (yield 93%) with m.p. 119-120° C. after recrystallization from tetrahydrofuran was obtained. I.r.: 1168, 965 (P—Ph), 1196 (P═O), 2384 (P—H), 1587 cm−1 (P—Ph). Anal. Calcd. for C12H9O2P: C, 66.67; H, 4.17; O, 14.81; P, 14.35. Found: C, 66.64; H, 4.31; O, 14.59; P, 14.66. MS, m/z: 216 (100, M+).

Aufarbeitung

temperatureThe temperature was slowly increased from 106 to 160° C. until the dehydration

Quellen und Nachweise

ORD-Eintrag: ord-7e4df92fbff84925b7340641c3d2c908
Quelldatensatz: uspto-grants-2001_09
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US06291626B1

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