Hydrochloric Acid → HCID 67254699, compound
Reaction equation
C([O:3][C:4]([CH:6]1[CH:11]([CH3:12])[O:10][CH2:9][CH2:8][NH:7]1)=[O:5])C.[OH-].[K+].Cl>CO.O>[CH3:12][CH:11]1[O:10][CH2:9][CH2:8][NH:7][CH:6]1[C:4]([OH:5])=[O:3]Participants
6
Reactant 3
Product 1
Reagents, catalysts & solvents 2
Conditions
- Temperature
- 75 °C
Procedure
To a solution of 2-methyl-morpholine-3-carboxylic acid ethyl ester (Comp. No. 27) (0.180 g, 1.039 mmol) in methanol (4 ml) was added water (2 ml) and potassium hydroxide (0.291 g, 5.195 mmol). The resulting mixture was heated to 75° C. until the color turned to red. The mixture was allowed to cool to room temperature, diluted with water and acidified to pH=1 with aqueous hydrochloric acid (2 M). The solution was washed with a mixture of dichloromethane and isopropanol (3:1) and freeze-dried. The resulting white solid was used in the next step without further purification. LC/MS (method 7): Rt=0.11 min; m/z=146.20 (M+H+).
Workup
- temperatureto cool to room temperature
- washThe solution was washed with a mixture of dichloromethane and isopropanol (3:1)
- customfreeze-dried
- customThe resulting white solid was used in the next step without further purification
Sources & evidence
- ORD record
- ord-3f8a4fb8fed0457a859f60a601f85c11
- Source dataset
- uspto-grants-2016_03
- Patent number
- US09284333B2
Reaction notes
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