Hydrochloric Acid → 5.6-Dichloro-3-(2-(S)-azetidinylmethoxy)pyridine hydrochloride

HRID 1416663노트

반응식

HRID 1416663 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([O:9][CH2:10][C@@H:11]2[CH2:14][CH2:13][NH:12]2)[CH:5]=[N:6][C:7]=1[Cl:8].Cl>CCOCC>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([O:9][CH2:10][C@@H:11]2[CH2:14][CH2:13][NH:12]2)[CH:5]=[N:6][C:7]=1[Cl:8]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 102633765,6-Dichloro-3-(2-(S)-azetidinylmethoxy)pyridine

생성물 1

HCID 213097065.6-Dichloro-3-(2-(S)-azetidinylmethoxy)pyridine hydrochloride수율 162.2%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

The compound from step 109c (338 mg, 1.45 mmol) was slurried in ether (15 mL), and ether saturated with HCl gas was added. Solvent was removed and the remaining white solid was recrystallized from methanol/Et2O to give 317 mg of short white needles, 81% yield. m.p. =181-182° C. MS (CI) m/e 233 (M+H)+. 1H NMR (20, 300 MHz) δ: 8.13 (d, J=2.9 Hz, 1H), 7.79 (d, J=2.9 Hz, 1H), 4.99-4.91 (m, 1H), 4.44 (d, J=4.4 Hz, 2H), 4.21-4.03 (m, 2H), 2.74-2.65 (m, 2H). Anal. calc. for C9H11Cl3N2O: C, 40.10; H, 4.11; N, 10.39; Found: C, 39.89; H, 4.08; N, 10.25.

후처리

  1. customSolvent was removed
  2. customthe remaining white solid was recrystallized from methanol/Et2O

출처 및 근거

ORD 기록
ord-e9b3114c4f9b48da8a8bc8f9380b0853
출처 데이터셋
uspto-grants-1999_06
특허 번호
US05914328

반응 노트

불러오는 중…