Methyl iodide → HCID 178437540, compound
Reaction equation
CI.[CH2:3]([C:5]1[S:6][C:7]2[CH:14]=[CH:13][C:12]3[CH:15]=[C:16]([CH3:19])[CH:17]=[CH:18][C:11]=3[CH:10]([C:20]3[C:21](=[S:27])[NH:22][C:23](=[O:26])[NH:24][CH:25]=3)[C:8]=2[N:9]=1)[CH3:4].[C:28](=O)(O)[O-].[Na+]>C(O)C.O>[CH2:3]([C:5]1[S:6][C:7]2[CH:14]=[CH:13][C:12]3[CH:15]=[C:16]([CH3:19])[CH:17]=[CH:18][C:11]=3[CH:10]([C:20]3[C:21]([S:27][CH3:28])=[N:22][C:23](=[O:26])[NH:24][CH:25]=3)[C:8]=2[N:9]=1)[CH3:4]Participants
6
Reactant 3
Product 1
Reagents, catalysts & solvents 2
Procedure
Methyl iodide (0.044 ml) was added to a stirred solution of the product from example 31 step (v) (0.250 g) and sodium bicarbonate (0.057 g) in ethanol (5 ml) and water (3 ml). After 3 h the reaction mixture was partitioned between ethyl acetate and water. The organic phase was washed with water, dried (MgSO4) and evaporated under reduced pressure. Purification was by trituration with ethyl acetate and isohexane.
Workup
- customAfter 3 h the reaction mixture was partitioned between ethyl acetate and water
- washThe organic phase was washed with water
- dry with materialdried (MgSO4)
- customevaporated under reduced pressure
- customPurification
Sources & evidence
- ORD record
- ord-4f3e85d924814e2aada917635b64268b
- Source dataset
- uspto-grants-2001_04
- Patent number
- US06218376B1
Reaction notes
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