Hydrochloric Acid → HCID 18934765, 화합물

HRID 3285노트

반응식

HRID 3285 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]23[CH2:14][CH2:13][CH2:12][N:11]2[CH2:10][CH2:9][CH2:8]3)[CH:2]=1.CCOCC.[ClH:20]>C(Cl)Cl>[ClH:20].[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]23[CH2:8][CH2:9][CH2:10][N:11]2[CH2:12][CH2:13][CH2:14]3)[CH:2]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 104199907a-(3-Pyridinyl)-hexahydro-1h-pyrrolizine

생성물 1

HCID 18934765HCID 18934765, 화합물수율 81%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

7a-(3-pyridinyl)-hexahydro-1H-pyrrolizine (from step 3a, 125 mg, 0.66 mmol) was dissolved in CH2Cl2 (15 mL) and Et2O saturated with HCl (g) was added dropwise. The solvent was removed, and the remaining solid was triturated with CH2Cl2 (2×) to afford a hygroscopic yellow solid (140 mg, 81%). MS (CI/NH3) m/e: 189 (M+H)+. 1H NMR (D2O, 300 MHz) δ2.13-2.29 (m, 2H), 2.32-2.43 (m, 2H), 2.48-2.69 (m, 4H), 3.40-3.49 (m, 2H), 3.83-3.92 (m, 2H), 7.92 (dd, J=8.5, 5.5 Hz, 1H), 8.43 (ddd, J=8.5, 2.6, 1.4 Hz, 1H), 8.75 (dd, J=5.5, 1.4 Hz, 1H), 8.88 (d, J=2.6 Hz, 1H). Anal. Calcd for C12H18Cl2N2.0.5H2O: C, 53.34; H, 7.09; N, 10.37. Found: C, 53.28; H, 6.96; N, 10.22.

후처리

  1. customThe solvent was removed
  2. customthe remaining solid was triturated with CH2Cl2 (2×)

출처 및 근거

ORD 기록
ord-4a0b85df694b48eb9e5baebab0e7dade
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733912

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