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

HRID 1416663ノート

反応式

HRID 1416663 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-e9b3114c4f9b48da8a8bc8f9380b0853
出典データセット
uspto-grants-1999_06
特許番号
US05914328

反応ノート

読み込み中…