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

HRID 645345ノート

反応式

HRID 645345 の反応式
[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

参加物

4

反応物 2

HCID 11776TriphenylphosphineHCID 5207261-Bromo-5-methylhexane

生成物 1

HCID 44126650(5-Methylhexyl)(triphenyl)phosphanium bromide収率 81%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of 25 (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.

後処理

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

出典と根拠

ORDレコード
ord-ca6bb68051324fe1a65f370be0692836
出典データセット
uspto-grants-2010_04
特許番号
US07704981B2

反応ノート

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