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

HRID 3304ノート

反応式

HRID 3304 の反応式
[CH2:1]([C:4]1[CH:8]=[C:7]([C:9]23[CH2:16][CH2:15][CH2:14][N:13]2[CH2:12][CH2:11][CH2:10]3)[O:6][N:5]=1)[CH2:2][CH3:3].[ClH:17]>CCOCC>[ClH:17].[CH2:1]([C:4]1[CH:8]=[C:7]([C:9]23[CH2:10][CH2:11][CH2:12][N:13]2[CH2:14][CH2:15][CH2:16]3)[O:6][N:5]=1)[CH2:2][CH3:3]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 189347247a-(3-propyl-5-isoxazolyl)-hexahydro-1H-pyrrolizine

生成物 1

HCID 189347587a-(3-Propyl-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-propyl-5-isoxazolyl)-hexahydro-1H-pyrrolizine (265 mg, 1.30 mmol, from step 14a) was dissolved in Et2O, and Et2O saturated with HCl (g) was added. The solvent was removed, and the precipitate was triturated with Et2O and dried to afford the title compound as a free flowing white powder. mp 97°-98° C. MS (NH3 /CI): m/z 207 (M+H+); 1H NMR (D2O, 300 MHz) δ0.92 (t, J=7.5 Hz, 3H), 1.63-1.75 (m, 2H), 2.20-2.40 (m, 6H), 2.59-2.71 (m, 4H), 3.30-3.38 (m, 2H), 3.70-3.78,(m, 2H), 6.65 (s, 1H); MS (CI/NH3) m/z: 221 (M+H)+.Anal. Calcd for C13H20N2O.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 triturated with Et2O
  3. customdried

出典と根拠

ORDレコード
ord-402839b675474c22a8bd5c354e9adae4
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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