Hydrochloric Acid → HCID 67432550, compound
Reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[N:9]([C@H:25]([CH3:28])[CH2:26][OH:27])[C:10]2[C:15]([N:16]=1)=[C:14]([N:17]1[CH2:22][CH2:21][N:20]([CH3:23])[CH2:19][CH2:18]1)[N:13]=[C:12]([CH3:24])[N:11]=2.Cl.O1CCOCC1>C(OCC)C>[ClH:1].[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[N:9]([C@H:25]([CH3:28])[CH2:26][OH:27])[C:10]2[C:15]([N:16]=1)=[C:14]([N:17]1[CH2:18][CH2:19][N:20]([CH3:23])[CH2:21][CH2:22]1)[N:13]=[C:12]([CH3:24])[N:11]=2Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
Dissolve (2R)-2-[8-(2-chlorophenyl)-2-methyl-6-(4-methylpiperazin-1-yl)purin-9-yl]propan-1-ol (15.29 g, 38.14 mmol) in diethyl ether (114 mL) in a 250 mL round bottom flask, fitted with nitrogen inlet, and treat with 4 N hydrogen chloride in dioxane (9.53 mL, 38.14 mmol). Stir at room temperature for 2.5 h and then collect the solids by vacuum filtration. Wash with diethyl ether (300 mL) and then dry under vacuum to afford the title compound (12.1 g). ES/MS m/z 401.2 (M+1−HCl).
Workup
- customfitted with nitrogen inlet
- customcollect the solids
- filtrationby vacuum filtration
- washWash with diethyl ether (300 mL)
- customdry under vacuum
Sources & evidence
- ORD record
- ord-9331a3a5fd81420d9bfd99d6a509b313
- Source dataset
- uspto-grants-2014_06
- Patent number
- US08759360B2
Reaction notes
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