Hydrochloric Acid → 7a-(3-Ethyl-5-isoxazolyl)-hexahydro-1h-pyrrolizine hydrochloride salt

HRID 3302

反応式

HRID 3302 の反応式
[CH2:1]([C:3]1[CH:7]=[C:6]([C:8]23[CH2:15][CH2:14][CH2:13][N:12]2[CH2:11][CH2:10][CH2:9]3)[O:5][N:4]=1)[CH3:2].[ClH:16]>CCOCC>[ClH:16].[CH2:1]([C:3]1[CH:7]=[C:6]([C:8]23[CH2:15][CH2:14][CH2:13][N:12]2[CH2:11][CH2:10][CH2:9]3)[O:5][N:4]=1)[CH3:2]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 189347517a-(3-ethyl-5-isoxazolyl)-hexahydro-1H-pyrrolizine

生成物 1

HCID 189347627a-(3-Ethyl-5-isoxazolyl)-hexahydro-1h-pyrrolizine hydrochloride salt

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

7a-(3-ethyl-5-isoxazolyl)-hexahydro-1H-pyrrolizine (265 mg, 1.30 mmol, from step 13b) was dissolved in Et2O, and Et2O saturated with HCl (g) was added. The solvent was removed, and the precipitate was recrystallized from methanol/ethanol to afford the title compound as a white solid: mp 139°-140° C.; 1H NMR D2O, 300 MHz) δ1.23 (t, J=7.5 Hz, 3H), 2.17-2.40 (m, 6H), 2.58-2.75 (m, 4H), 3.29-3.38 (m, 2H), 3.69-3.77 (m, 2H), 6.64 (s, 1H); MS (CI/NH3) m/z: 207 (M+H)+ ; Anal. Calcd for C12H18N2O.HCl: C, 59.38; H, 7.89; N, 11.54. Found: C, 59.44; H, 7.94; N, 11.48.

後処理

  1. customThe solvent was removed
  2. customthe precipitate was recrystallized from methanol/ethanol

出典と根拠

ORDレコード
ord-6a17fe06ca0a4559821af5872f757c00
出典データセット
uspto-grants-1998_03
特許番号
US05733912

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