Hydrochloric Acid → HCID 18934765、化合物

HRID 3285ノート

反応式

HRID 3285 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 18934765HCID 18934765、化合物収率 81%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-4a0b85df694b48eb9e5baebab0e7dade
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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