Pentane → Di-tert-butyl-trimethylsilylmethyl-phosphane

HRID 16925

反応式

HRID 16925 の反応式
[C:1]([P:5]([C:7]([CH3:10])([CH3:9])[CH3:8])Cl)([CH3:4])([CH3:3])[CH3:2].CCCCC.[CH3:16][Si:17]([CH2:20][Li])([CH3:19])[CH3:18].[Cl-].[NH4+]>C1COCC1>[C:1]([P:5]([C:7]([CH3:10])([CH3:9])[CH3:8])[CH2:16][Si:17]([CH3:20])([CH3:19])[CH3:18])([CH3:4])([CH3:3])[CH3:2]

参加物

6

反応物 4

HCID 8003PentaneHCID 25517Ammonium ChlorideHCID 139566Di-tert-butylchlorophosphineHCID 178418939HCID 178418939、化合物

生成物 1

HCID 12583313Di-tert-butyl-trimethylsilylmethyl-phosphane

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

50.00 g (0.277 mol) of Di-t-butylchlorophosphine, 304 ml of 1.0 M pentane solution of (trimethylsilylmethyl)lithium and 150 ml of THF) were refluxed under argon for 3 days. The reaction mixture was allowed to cool off to RT and an aqueous solution of ammonium chloride was added slowly. The organic phase was separated, and dried with magnesium sulfate. After removal of the solvent, the product was purified by distillation in vacuum. The yield of di-tert-butyl-trimethylsilanylmethyl-phosphane was 55.32 g (86%) with b.p. 50-52° C./0.5 mm. 31P NMR (C6D6)+20.05 ppm. 1H NMR (C6D6) 0.01 (s, 9H, SiMe3), 0.23 (d, 2H, 2JPH=5.34 Hz, P—CH2—SiMe3), 0.91 (s, 9H, Me3C), 0.93 (s, 9H, Me3C). Anal. Calcd. for C12H29PSi: C, 62.01; H, 12.58; P, 13.33. Found: C, 61.89; H, 12.53; P, 13.25.

後処理

  1. customThe organic phase was separated
  2. dry with materialdried with magnesium sulfate
  3. customAfter removal of the solvent
  4. distillationthe product was purified by distillation in vacuum

出典と根拠

ORDレコード
ord-f020141d60174cacaa5888e5bc63f7cc
出典データセット
uspto-grants-2010_06
特許番号
US07737277B2

関連ノート

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