반응 #43561

ord-716e3510a0784031b618357edaf011b3

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출the aqueous layer was extracted with CH2Cl2 (50 mL×3)
  2. 2
    추출extracted with ethyl acetate (50 mL×3)
  3. 3
    건조The combined ethyl acetate fractions were dried over MgSO4
  4. 4
    여과filtered
  5. 5
    기타evaporated

실험 절차

4,4-Dimethyl-pentanoic acid methyl ester (7.0 g, 48.5 mmol, 1.0 eq.) was treated with a solution of NaOH (4.0 g, 100 mmol, 2.1 eq.) in water (5 mL). The homogeneous solution was allowed to stir for 4-5 hours. The reaction was diluted with CH2Cl2 and the aqueous layer was extracted with CH2Cl2 (50 mL×3). The aqueous layer was acidified with 6M HCl to pH˜1.5 and extracted with ethyl acetate (50 mL×3). The combined ethyl acetate fractions were dried over MgSO4, filtered and evaporated to provide 4,4-dimethyl-pentanoic acid (5.35 g, 41.1 mmol, 85%) as a colorless oil: 1H NMR (CDCl3, 400 MHz) δ 0.89 (s, 9H), 1.53-1.57 (m, 2H), 2.26-2.30 (m, 2H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07732449B2uspto-grants-2010_06