Sodium borohydride → HCID 21821162, compound
Reaction equation
[I-].[CH3:2][N+:3]1[CH2:8][CH2:7][C:6]2[CH:9]=[CH:10][S:11][C:5]=2[C:4]=1[CH3:12].[BH4-].[Na+]>CO>[CH3:2][N:3]1[CH2:8][CH2:7][C:6]2[CH:9]=[CH:10][S:11][C:5]=2[CH:4]1[CH3:12]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
A mixture of 7.2 g (24 mmol) 6,7-dimethyl-4,5-dihydro-thieno[2,3-c]pyridinium iodide and 80 ml of methanol is mixed batchwise 1.87 g (49 mmol) NaBH4 while cooling with an ice bath (vigorous release of gas). The mixture is stirred for another 1.5 h, concentrated, mixed with sat. NaHCO3 solution and extracted 3× with methylene chloride. The organic phases are dried on NaSO4, filtered and concentrated.
Workup
- temperaturewhile cooling with an ice bath (vigorous release of gas)
- concentrationconcentrated
- additionmixed with sat. NaHCO3 solution
- extractionextracted 3× with methylene chloride
- customThe organic phases are dried on NaSO4
- filtrationfiltered
- concentrationconcentrated
Sources & evidence
- ORD record
- ord-12e7451a4b9d44f4b2ca88fcf1719d21
- Source dataset
- uspto-grants-2012_11
- Patent number
- US08309542B2
Reaction notes
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