Triphenylphosphine → (5-Methylhexyl)(triphenyl)phosphanium bromide

HRID 1992250노트

반응식

HRID 1992250 반응식
[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][CH:6]([CH3:8])[CH3:7].[C:9]1([P:15]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>C1(C)C=CC=CC=1>[Br-:1].[CH3:7][CH:6]([CH3:8])[CH2:5][CH2:4][CH2:3][CH2:2][P+:15]([C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1)([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

참가 물질

4

반응물 2

HCID 11776TriphenylphosphineHCID 5207261-Bromo-5-methylhexane

생성물 1

HCID 44126650(5-Methylhexyl)(triphenyl)phosphanium bromide수율 81%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of 19 (2.30 g; 12.8 mmol) and triphenylphosphine (3.70 g; 14.1 mmol) was refluxed in toluene (12 mL) for 20 h. Then solvent was removed and the resulting crystal was washed with toluene (3 mL) and diethyl ether (3 mL) to give 4.57 g (10.4 mmol; 81% yield) of 10. m.p. 227-228° C.; 1H NMR (500 MHz, CD3CN) δ 0.82 (6H, d, J=6.6 Hz), 1.16 (2H, m), 1.42-1.52 (3H, m), 1.59 (2H, m), 3.30 (2H, m), 7.72 (12H, m), 7.85 (3H, m); 13C NMR (125 MHz, CD3CN) δ 22.7, 23.2, 28.4, 28.8, 28.9, 38.6, 131.2, 131.3, 134.7, 134.7, 136.0.

후처리

  1. customThen solvent was removed
  2. washthe resulting crystal was washed with toluene (3 mL) and diethyl ether (3 mL)

출처 및 근거

ORD 기록
ord-88f7e0f34a46467e932ef547d03e565c
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07648972B2

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