Dichloro(diethylamino)phosphine → Cyclohexyl(diethylamino)chlorophosphine

HRID 979711

반응식

HRID 979711 반응식
[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]

참가 물질

3

반응물 2

HCID 2733289Dichloro(diethylamino)phosphineHCID 178478990HCID 178478990, 화합물

생성물 1

HCID 4368802Cyclohexyl(diethylamino)chlorophosphine수율 57.5%

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-97bc99cfccb84eb7bff4ad4cbe27f189
출처 데이터셋
uspto-grants-1987_05
특허 번호
US04668823

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