Hydrochloric Acid → HCID 67073212, compound
Reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][O:5][CH2:4][CH2:3]1.Cl.[CH2:9]([Cl:11])[Cl:10]>>[CH3:1][N:2]1[CH2:7][CH2:6][O:5][CH2:4][CH2:3]1.[CH2:9]([Cl:11])[Cl:10]Participants
4
Procedure
To a solution of crude G or G′ (1 eq.) in anhydrous DCM were added at 0° C. H (1.3 eq.), followed by N-methylmorpholine (2.2 eq.) dropwise over 15 sec. The reaction mixture was stirred at rt for 10 minutes and, the milky suspension was poured into 1 M HCl. The aqueous phase was extracted with DCM. The organic phases were combined, washed with 1 M NaOH, brine, dried over MgSO4 and evaporated to dryness. The crude compound was purified by silica gel chromatography to afford the desired product (R)-I.
Workup
- extractionThe aqueous phase was extracted with DCM
- washwashed with 1 M NaOH, brine
- dry with materialdried over MgSO4
- customevaporated to dryness
- customThe crude compound was purified by silica gel chromatography
Sources & evidence
- ORD record
- ord-5ccbc00c836947128cd22da9b795031a
- Source dataset
- uspto-grants-2016_08
- Patent number
- US09422299B2
Reaction notes
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