Dichloromethane → HCID 10607830, compound
Reaction equation
[CH3:1][S:2](Cl)(=[O:4])=[O:3].CC[N:8]([CH:12]([CH3:14])[CH3:13])[CH:9]([CH3:11])C.[Cl:15]CCl>>[Cl:15][CH2:14][C:12]1[N:8]([S:2]([CH3:1])(=[O:4])=[O:3])[CH:9]=[CH:11][CH:13]=1Participants
4
Procedure
At 0° C. methanesulfonyl chloride (136 μl) was added dropwise to a solution of the product of example 51b (205 mg) and DIPEA (307 μl) in dichloromethane (6 ml). After stirring for 30 min, the reaction mixture was diluted with dichloromethane (30 ml) and washed with ice water (30 ml), 10% HCl (30 ml) and sat. NaHCO3. The organic layer was separated, dried (MgSO4), filtered and concentrated in vacuo. Yield: 252 mg.
Workup
- washwashed with ice water (30 ml), 10% HCl (30 ml) and sat. NaHCO3
- customThe organic layer was separated
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
Sources & evidence
- ORD record
- ord-d5225a0cfb56414195f3a3b8b559c0f5
- Source dataset
- uspto-grants-2011_09
- Patent number
- US08022218B2
Reaction notes
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