Hydrochloric Acid → HCID 66662781, compound
Reaction equation
C(OC([N:8]1[CH2:17][CH2:16][C:15]2[C:10](=[CH:11][CH:12]=[C:13]([NH:18][C:19]([O:21][CH2:22][C:23]3[CH:28]=[C:27]([Cl:29])[CH:26]=[C:25]([Cl:30])[CH:24]=3)=[O:20])[CH:14]=2)[CH2:9]1)=O)(C)(C)C.Cl>C(O)CC.CC(O)C.C(OCC)C>[Cl:29][C:27]1[CH:28]=[C:23]([CH:24]=[C:25]([Cl:30])[CH:26]=1)[CH2:22][O:21][C:19](=[O:20])[NH:18][C:13]1[CH:14]=[C:15]2[C:10](=[CH:11][CH:12]=1)[CH2:9][NH:8][CH2:17][CH2:16]2Participants
6
Reactant 2
Product 1
Reagents, catalysts & solvents 3
Procedure
Starting material 46 (170 mg, 0.4 mmol) was dissolved in 5 ml propanol. Then 1 ml HCl in 2-propanol (5-6 N) was added and the mixture was stirred over night at ambient temperature. The reaction mixture was then diluted with diethyl ether, concentrated in vacuo and stirred with diethyl ether, repeatedly decanting. Finally the solid residue was filtered off and dried in vacuo at 45° C. Thus the desired product 47 was isolated as brownish crystals (46 mg, 0.1 mmol, 35%).
Workup
- concentrationconcentrated in vacuo
- stirringstirred with diethyl ether
- customrepeatedly decanting
- filtrationFinally the solid residue was filtered off
- customdried in vacuo at 45° C
Sources & evidence
- ORD record
- ord-6856684df112426cacbecfb50f1e9b3f
- Source dataset
- uspto-grants-2012_12
- Patent number
- US08329907B2
Reaction notes
Loading…