Hydrochloric Acid → bis(3-methylphenyl)phosphinic acid

反応式

Br[C:2]1[CH:3]=[C:4]([CH3:8])[CH:5]=[CH:6][CH:7]=1.[Mg].C(N(CC)[P:13](Cl)([O-:15])=[O:14])C.Cl>>[C:4]1([CH3:8])[CH:5]=[CH:6][CH:7]=[C:2]([P:13]([C:2]2[CH:3]=[C:4]([CH3:8])[CH:5]=[CH:6][CH:7]=2)(=[O:14])[OH:15])[CH:3]=1

参加物

反応物 4

HCID 313Hydrochloric Acid

HCID 115603-Bromotoluene

HCID 5462224Magnesium

HCID 20059535HCID 20059535、化合物

生成物 1

HCID 262047bis(3-methylphenyl)phosphinic acid

実験手順

That is, m-bromotoluene (II) is reacted with metallic magnesium to prepare a Grignard reagent (III) which is then condensed with N,N-diethylamidochlorophosphate (IV) obtained by the process described in G. M. Kosolapoff et al., J. Am. Chem. Soc., Vol. 71, pp. 369-370 (1949), followed by hydrolysis with hydrochloric acid to obtain di-(m-tolyl)phosphinic acid (V). The compound (V) is reacted with thionyl chloride. After removing excess thionyl chloride, the reaction mixture is recrystallized from a mixed solution of benzene and hexane to obtain di-(m-tolyl)phosphonyl chloride (VI).

後処理

customobtained by the process

出典と根拠

ORDレコード: ord-27b4d8d2ff854867ae341c5de0db50f5
出典データセット: uspto-grants-1991_04
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US05012002

反応ノート

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