HCID 86688406, compound → HCID 86688405, compound
Reaction equation
[CH3:1][N:2]1[C:10]([NH:11][C:12]([NH:14]C(=O)C2C=CC=CC=2)=[S:13])=[C:9]2[C:4]([CH2:5][CH2:6][CH2:7][CH2:8]2)=[N:3]1>[OH-].[Na+]>[CH3:1][N:2]1[C:10]([NH:11][C:12]([NH2:14])=[S:13])=[C:9]2[C:4]([CH2:5][CH2:6][CH2:7][CH2:8]2)=[N:3]1Participants
3
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 90 °C
Procedure
A suspension of compound 125 (3.1 g, 9.5 mmol) in 30 mL of 5% NaOH aqueous solution was stirred in an oil bath of 90° C. for 8 hrs and cooled down to room temperature. Ice was added while stirring to the reaction mixture. The resulting suspension was filtered, and the cake was washed with cold water (10 mL×3) and further dried in vacuo to afford the desired product 113 as an off-white powder.
Workup
- temperaturecooled down to room temperature
- additionIce was added
- stirringwhile stirring to the reaction mixture
- filtrationThe resulting suspension was filtered
- washthe cake was washed with cold water (10 mL×3)
- customfurther dried in vacuo
Sources & evidence
- ORD record
- ord-e482b2756f2e469ea40eee7561bca413
- Source dataset
- uspto-grants-2016_08
- Patent number
- US09403815B2
Reaction notes
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