Hydrochloric Acid → HCID 86750808、化合物

HRID 1780345ノート

反応式

HRID 1780345 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 ether, and the solid was dried under high vacuum to afford the title compound (99.2 mg). mp 230° C. MS (CDI/NH3) m/z 291/293 (M+H)+. 1 H 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 ether
  3. customthe solid was dried under high vacuum

出典と根拠

ORDレコード
ord-4c9d282246274d83a6000e020f8af454
出典データセット
uspto-grants-1997_05
特許番号
US05629325

反応ノート

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