Benzyl 2-(di-tert-butoxyphosphoryloxy)ethylcarbamate → 2-Aminoethyl di(tert-butyl) phosphate

HRID 2238447

반응식

HRID 2238447 반응식
[C:1]([O:5][P:6]([O:13][CH2:14][CH2:15][NH:16]C(=O)OCC1C=CC=CC=1)([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:7])([CH3:4])([CH3:3])[CH3:2]>CO.[Pd]>[P:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])([O:8][C:9]([CH3:10])([CH3:12])[CH3:11])([O:13][CH2:14][CH2:15][NH2:16])=[O:7]

참가 물질

4

반응물 1

HCID 68635482Benzyl 2-(di-tert-butoxyphosphoryloxy)ethylcarbamate

생성물 1

HCID 862404572-Aminoethyl di(tert-butyl) phosphate수율 79%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A solution of 225 (1.17 g, 3.02 mmol) in MeOH (30 mL) with Pd/C (5%, 0.21 g) was hydrogenated at 50 psi for 2.5 h. The mixture was filtered through Celite, washing with MeOH, and the filtrate was evaporated. The residue was dissolved in CH2Cl and the solution was filtered once more, then evaporated to give 2-aminoethyl di(tert-butyl) phosphate (226) (604 mg, 79%) as a colourless oil: 1H NMR [CDCl3] δ 4.01-3.94 (m, 2H), 2.96-2.90 (m, 2H), 1.58 (br s, 2H), 1.49 (s, 18H). HRMS (FAB) calcd. for C10H25NO4P (MH+) m/z 254.1521, found 254.1519.

후처리

  1. filtrationThe mixture was filtered through Celite
  2. washwashing with MeOH
  3. customthe filtrate was evaporated
  4. dissolutionThe residue was dissolved in CH2Cl
  5. filtrationthe solution was filtered once more
  6. customevaporated

출처 및 근거

ORD 기록
ord-1822e72c026842a18ad49259fc79ee86
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07718688B2

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