Hydrochloric Acid → 7a-(4-Methyl-3-pyridinyl)-hexahydro-1h-pyrrolizine dihydrochloride salt

HRID 3330노트

반응식

HRID 3330 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[C:8]12[CH2:15][CH2:14][CH2:13][N:12]1[CH2:11][CH2:10][CH2:9]2.[ClH:16]>CCOCC>[ClH:16].[ClH:16].[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[C:8]12[CH2:15][CH2:14][CH2:13][N:12]1[CH2:11][CH2:10][CH2:9]2

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 189347417a-(4-methyl-3-pyridinyl)-hexahydro-1H-pyrrolizine

생성물 1

HCID 189347407a-(4-Methyl-3-pyridinyl)-hexahydro-1h-pyrrolizine dihydrochloride salt수율 61%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

7a-(4-methyl-3-pyridinyl)-hexahydro-1H-pyrrolizine (37 mg, 0.18 mmol) was dissolved in Et2O, and Et2O saturated with HCl (g) was added. The solvent was removed, and the solid was triturated with Et2O and dried to afford the title compound as a white solid (26.2 mg, 61%): mp 244°-247° C.; 1H NMR D2O, 300 MHz) δ2.01-2.16 (m, 2H), 2.27-2.52 (m, 4H), 2.65 (s, 3H), 2.65-2.78 (m, 2H), 3.45-3.54 (m, 2H), 3.87-3.96 (m, 2H), 7.75 (d, J=5.6 Hz, 1H), 8.49 (s, 1H), 8.55 (d, J=5.6 Hz, 1H); MS (CI/NH3): m/z 203 (M+H+). Anal. Calcd for C13H18N2.2 HCl: C, 56.73; H, 7.32; N, 10.18. Found: C, 56.94; H. 7.24; N, 9.99.

후처리

  1. customThe solvent was removed
  2. customthe solid was triturated with Et2O
  3. customdried

출처 및 근거

ORD 기록
ord-9f0d302e51834ee5ae59f2e30cfe7ffc
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733912

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