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

HRID 3330ノート

反応式

HRID 3330 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-9f0d302e51834ee5ae59f2e30cfe7ffc
出典データセット
uspto-grants-1998_03
特許番号
US05733912

反応ノート

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