ジ(1‐アダマンチル)‐N‐ブチルホスフィン 化学特性,用途語,生産方法
物理的性質
Butyldi-1-adamantylphosphine is a white to yellow solid with a melting
point of 100°C and an estimated boiling point of 449.6±12.0°C. Store at
room temperature, it is air sensitive.
使用
suzuki reaction
一般的な説明
Sold in collaboration with Solvias AG
合成
Phosphonium salt (2.2 mmol) was added to a cooled solution (- 78 ??C) of
Et3N
(4.44 g, 44 mmol) in di-n-butyl ether (20 mL). The reaction mixture was
stirred at -78 ??C for 5 h and then allowed to warm gradually to r.t.
The solvent was removed under vacuum and the residue was dissolved in
degassed EtOH (5 mL). After stirring for 15 min, the solid was filtered
off and dried to yield the desired phosphine, which can be further
purified by crystallization from EtOH. Butyldi-1-adamantylphosphine,
yield 90%.
31P NMR (C6D6)|?: 24.9. Mp 108-110??C. IR (KBr): 3425 (m, br),
2952 (s), 2847 (s), 2847 (s), 2675 (w), 1446 cm-1 (m). 1H NMR (250 MHz,
C6D6): |? = 0.96 (3 H, t, 3JH, H = 7.3 Hz, CH3), 1.35-2.03 (36 H, m,
adamantyl-30H, butyl-6H). 13C NMR (62 MHz, C6D6): |? = 41.3 (d, 2JC,P =
11.3 Hz, C-2), 37.4 (C-4), 36.1 (d, 1JC,P = 23.5 Hz, C-1), 33.9 (d,
1JC,P = 26.2 Hz, butyl-|á -CH2), 29.1 (d, 3JC,P = 7.6 Hz, C-3), 24.9 (d,
2JC,P = 13.1 Hz, butyl-|? -CH2), 17.1 (d, 3JC,P = 21.6 Hz, butyl-|? -CH2),
14.3 (butyl-CH3). MS (EI, 70 eV): m/z (%) = 358 (M+, 60), 135 (Ad+,
100).
ジ(1‐アダマンチル)‐N‐ブチルホスフィン 上流と下流の製品情報
原材料
準備製品