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

HRID 3302

반응식

HRID 3302 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-6a17fe06ca0a4559821af5872f757c00
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733912

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