반응 #67562

ord-b7e8c3d44885490494045fe7a410aca7

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축was concentrated to dryness
  2. 2
    기타After drying under vacuum

실험 절차

Compound 135 (272 mg, 0.335 mmol) was treated with a 50% v/v solution of TFA in CH2Cl2 (4 mL). After stirring for 3 hr the reaction mixture was concentrated to dryness and coevaporated with toluene. After drying under vacuum, acid 136 was obtained as a colorless liquid (304 mg, 120%) and was used without purification. 1H NMR (400 MHz, CDCl3) δ 1.25 (t, J=7.3, 3H), 1.32-1.37 (m, 12H), 1.70-1.81 (m, 4H), 1.93-2.02 (m, 2H), 2.13 (s, 3H), 2.20 (s, 3H), 2.20-2.29 (m, 2H), 2.47 (tt, J=5.8, 24.5, 1H), 2.57 (q, J=7.7, 2H), 2.74-2.81 (m, 1H), 2.87-2.93 (m, 1H), 3.01 (dd, J=6.2, 14.0, 1H), 3.15 (dd, J=5.5, 14.0, 1H), 3.66 (t, J=6.8, 2H), 4.14-4.22 (m, 8H), 4.75-4.80 (m, 1H), 6.12 (d, J=7.6, 1H), 6.67 (s, 1H), 7.06-7.09 (m, 2H), 7.14-7.24 (m, 3H): 31P (162 MHz, CDCl3) δ 24.35 (s, 1 P), 24.39 (s, 1 P).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08524691B2uspto-grants-2013_09