Glyoxal → 1,2-Dihydroxy-1,2-bis(diphenylphosphinyl)ethane

HRID 1388280노트

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HRID 1388280 반응식
[CH:1]([CH:3]=[O:4])=[O:2].[C:5]1([PH:11](=[O:18])[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1>C1C=CC=CC=1>[OH:2][CH:1]([P:11]([C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1)([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:18])[CH:3]([OH:4])[P:11]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)([C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=1)=[O:18]

참가 물질

4

반응물 2

HCID 7860GlyoxalHCID 254003Diphenylphosphine oxide

생성물 1

HCID 128292111,2-Dihydroxy-1,2-bis(diphenylphosphinyl)ethane수율 90%

시약·촉매·용매 1

HCID 241Benzene용매

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온도
40 °C

실험 절차

7.73 g of 30% aqeous glyoxal solution (40 mmols glyoxal), 16.17 g (80 mmols) of diphenylphosphine oxide and 40 ml of benzene were introduced into a round bottom flask. The initial pH of the reaction mixture was heated for 30 min with a water bath at 40° C. The precipitated white product was separated by filtration and weighed 16.64 g (90% yield) m.p. 211°-214° C. After recrystallization from dimethylsulfoxide-acetonitrile 3:2, V:V gave a sample of 1,2-dihydroxy-1,2-bis(diphenylphosphinyl)ethane m.p. 216°-217° C. Anal. Calcd for C26H24O4P2 : C,67.53; H, 5.23. Found: C,67.42; H, 5.34.

후처리

  1. customThe precipitated white product was separated by filtration
  2. customAfter recrystallization from dimethylsulfoxide-acetonitrile 3:2, V

출처 및 근거

ORD 기록
ord-e8b56d08583f4cc3a4eb391f2d7144d9
출처 데이터셋
uspto-grants-1984_02
특허 번호
US04431596

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