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

HRID 1596698

반응식

HRID 1596698 반응식
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

참가 물질

3

반응물 1

HCID 180000302-(2-Hydroxyphenyl)phenylphosphonic acid

생성물 1

HCID 37314CID 37314수율 93%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
106 °C

실험 절차

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+).

후처리

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

출처 및 근거

ORD 기록
ord-7e4df92fbff84925b7340641c3d2c908
출처 데이터셋
uspto-grants-2001_09
특허 번호
US06291626B1

연결된 노트

불러오는 중…