반응 #70160

ord-ce316869c633465c80d5bba21a1b3c64

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도at reflux for 18 hr
  2. 2
    온도cooled
  3. 3
    농축concentrated to a brown solid
  4. 4
    여과filtered
  5. 5
    기타to yield 450 mg (75%) of Ex 5-Step 1 product as a tan colored solid

실험 절차

4-[3-(4-Fluorophenyl)-1-methyl-1H-pyrazol-4-yl]furo[3,4-b]pyridin-5(7H)-one (Example 1, step 5, 472 mg, 1.46 mmol) and benzyl amine (0.167 mL, 1.53 mmol) in acetic acid (4.7 mL) were heated at reflux for 18 hr, cooled and then concentrated to a brown solid. This material was stirred with diethyl ether (20 mL) for 10 min and then filtered to yield 450 mg (75%) of Ex 5-Step 1 product as a tan colored solid: LCMS m/z 413.5 (M+1); 1H NMR (400 MHz, CDCl3) δ 8.57 (d, J=5.2, 1H), 8.15 (s, 1H), 7.26-7.42 (m, 7H), 7.13 (d, J=5.3, 1H), 7.01 (dd, J=8.6, 8.6, 2H), 4.87 (s, 2H), 4.00 (s, 3H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08536164B2uspto-grants-2013_09