반응 #1929093

ord-c9f8afe2c63c40e4ab28f6e1a1797cf1

반응 방정식

CCOP(=O)(OCC)C(CC(=O)OC(C)(C)C)P(=O)(OCC)OCC
Ester
CCOP(=O)(OCC)C(CC(=O)OC(C)(C)C)P(=O)(OCC)OCC
t-Butyl 3,3-bis(diethylphosphono)propanoate
CCOP(=O)(OCC)C(CC(=O)O)P(=O)(OCC)OCC
Acid 41
CCOP(=O)(OCC)C(CC(=O)O)P(=O)(OCC)OCC
3,3-bis(diethylphosphono)propanoic acid

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축concentrated under reduced pressure
  2. 2
    기타Crude acid 41 was purified by flash chromatography (gradient elution 100% ethyl acetate-10% methanol/ethyl acetate)

실험 절차

Ester 40 (2.1 g, 5.2 mmol) was stirred in TFA (12 mL) for 2.5 min and concentrated under reduced pressure. Crude acid 41 was purified by flash chromatography (gradient elution 100% ethyl acetate-10% methanol/ethyl acetate). Acid 41 was obtained as a white solid (1.35 g, 75%). 1H NMR (400 MHz, CDCl3) δ 1.28-1.39 (m, 12H), 2.86 (dt, J=16.1, 6.3, 2H), 3.12 (tt, J=24.0, 6.3, 1H), 4.13-4.26 (m, 8H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08946144B2uspto-grants-2015_02