Pentane → Di-tert-butyl-trimethylsilylmethyl-phosphane

HRID 16925

반응식

HRID 16925 반응식
[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]

참가 물질

6

반응물 4

HCID 8003PentaneHCID 25517Ammonium ChlorideHCID 139566Di-tert-butylchlorophosphineHCID 178418939HCID 178418939, 화합물

생성물 1

HCID 12583313Di-tert-butyl-trimethylsilylmethyl-phosphane

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f020141d60174cacaa5888e5bc63f7cc
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737277B2

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