Hydrochloric Acid → HCID 86750808、化合物

HRID 2305128ノート

反応式

HRID 2305128 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([O:9][CH2:10][C@H:11]2[CH2:15][CH2:14][CH2:13][N:12]2C(OC(C)(C)C)=O)[CH:5]=[N:6][C:7]=1[Cl:8].[ClH:23]>O1CCOCC1>[ClH:8].[ClH:23].[Br:1][C:2]1[CH:3]=[C:4]([O:9][CH2:10][C@H:11]2[CH2:15][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 22872666HCID 22872666、化合物

生成物 1

HCID 86750808HCID 86750808、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

5-bromo-6-chloro-3-(1-BOC-2-(R)-pyrrolidinylmethoxy)pyridine from step 69a (150 mg) was stirred with HCl in dioxane (3 mL) at room temperature for 16 hours. The precipitate formed was triturated with Et2O, and the solid was dried under high vacuum to afford the title compound (99.2 mg). mp 230° C. MS (CI/NH3) m/z 291/293 (M+H)+. 1H NMR (D2O, 300 MHz) δ: 1.89-2.02 (m, 1h), 2.05-2.21 (m, 2H), 2.21-2.35 (m, 1H), 3.42 (t, J=7.2 Hz, 2H), 4/12 (m, 1H), 4.25 (dd, J=7.8, 10.5 Hz, 1H), 4.47 (dd, J=3.2, 10.5 Hz, 1H), 7.90 (d, J=2.7 Hz, 1H), 8.13 (d, J=2.7 Hz, 1H). Anal. Calcd for C10H12N2OBrCl.2 HCl: C, 36.61; H, 3.99; N, 8.54. Found: C, 36.69; H, 3.91; N, 8.41. [α]25D=−14.80° (c 0.25, MeOH).

後処理

  1. customThe precipitate formed
  2. customwas triturated with Et2O
  3. customthe solid was dried under high vacuum

出典と根拠

ORDレコード
ord-c881b243bcca4eac9e217eb7cd376ef9
出典データセット
uspto-grants-2002_08
特許番号
US06437138B1

反応ノート

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