Dichloro(diethylamino)phosphine → Cyclohexyl(diethylamino)chlorophosphine

HRID 979711

反応式

HRID 979711 の反応式
[N:1]([P:6]([Cl:8])Cl)([CH2:4][CH3:5])[CH2:2][CH3:3].[CH:9]1([Mg]Cl)[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1>>[CH2:4]([N:1]([P:6]([CH:9]1[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1)[Cl:8])[CH2:2][CH3:3])[CH3:5]

参加物

3

反応物 2

HCID 2733289Dichloro(diethylamino)phosphineHCID 178478990HCID 178478990、化合物

生成物 1

HCID 4368802Cyclohexyl(diethylamino)chlorophosphine収率 57.5%

実験手順

U.S. Pat. No. 2,934,564 relates to compounds of the general formula R2PX wherein R represents an alkyl or aryl group and X represents chlorine, bromine or iodine. For example, the reaction of Me2NPCl2 (0.42 mole) with p-tolylmagnesium bromide (0.84 mole) produces dimethylamino-di-p-tolylphosphine. The isolated dimethylamino-di-p-tolylphosphine (31.88 mmoles) was treated with 1428 cc (63.75 mmoles) of anhydrous HCl yielding di-p-tolylchlorophosphine, which was purified by distillation. Similarly, Burg, et al. (J.A.C.S. 80, 1107-09, 1958) disclose the preparation of chlorodimethylphosphine from Me2NPCl2 and suggest the viability of a Grignard route to R2PR'-type phosphines. K. Issleib, et al. (Chem. Berichte 29, 2682-3008, 1959) have shown that Et2NPCl2 (Et=ethyl) and cyclohexylmagnesium chloride react in a 1:1.25 molar ratio to form diethylaminocyclohexylchlorophosphine in 57.5% yield. The authors suggest this reaction can be exploited to prepare unsymmetrical chlorophosphines of the type RR'PCl, but no mention is made of the possibility of further reaction to unsymmetrical tertiary phosphines of the type RR'R"P.

後処理

  1. distillationwas purified by distillation
  2. customthe preparation of chlorodimethylphosphine from Me2NPCl2
  3. customreact in a 1

出典と根拠

ORDレコード
ord-97bc99cfccb84eb7bff4ad4cbe27f189
出典データセット
uspto-grants-1987_05
特許番号
US04668823

関連ノート

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