Hydrochloric Acid → HCID 18704217, compound
Reaction equation
C([O:4][CH2:5][C:6]#[C:7][CH2:8][N:9]1[C:13]([CH2:16][F:17])([CH2:14][F:15])[C:12](=[O:18])[N:11]([C:19]2[CH:26]=[CH:25][C:22]([C:23]#[N:24])=[C:21]([C:27]([F:30])([F:29])[F:28])[CH:20]=2)[C:10]1=[O:31])(=O)C.CO.Cl.C(=O)(O)[O-].[Na+]>C(OCC)(=O)C>[F:15][CH2:14][C:13]1([CH2:16][F:17])[C:12](=[O:18])[N:11]([C:19]2[CH:26]=[CH:25][C:22]([C:23]#[N:24])=[C:21]([C:27]([F:30])([F:29])[F:28])[CH:20]=2)[C:10](=[O:31])[N:9]1[CH2:8][C:7]#[C:6][CH2:5][OH:4]Participants
6
Reactant 4
Product 1
Reagents, catalysts & solvents 1
Procedure
1 g of the product obtained in Stage 3 above, 18 ml of methanol and 4.5 ml of 2N hydrochloric acid are introduced then left for one hour 30 minutes at 50° C. The reaction medium is then returned to ambient temperature, poured into 30 ml of sodium bicarbonate, extraction is carried out with ethyl acetate 3 times, the extracts are washed with salt water and dried. After chromatography on silica eluting with methylene chloride-acetone: 85-15, 780 mg of expected product (white crystals) is obtained. M.p.=131-132° C.
Workup
- customis then returned to ambient temperature
- washthe extracts are washed with salt water
- customdried
Sources & evidence
- ORD record
- ord-369cfb69a982487f98406206858780c5
- Source dataset
- uspto-grants-2000_07
- Patent number
- US06087509
Reaction notes
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