Hydrochloric Acid → HCID 86750808, 화합물

HRID 365846노트

반응식

HRID 365846 반응식
[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]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 22872666HCID 22872666, 화합물

생성물 1

HCID 86750808HCID 86750808, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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) δ1.89-2.02 (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).

후처리

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

출처 및 근거

ORD 기록
ord-aa066b2f17824c428018ea2b0c84dda2
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06127386

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