Water → 3,3-Dimethyl-1-phenylhex-5-en-2-one
Reaction equation
[CH3:1][C:2]([CH3:15])([CH2:12][CH:13]=[CH2:14])[CH:3]([OH:11])[CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.CCN(C(C)C)C(C)C.O>C(Cl)Cl.CS(C)=O>[CH3:1][C:2]([CH3:15])([CH2:12][CH:13]=[CH2:14])[C:3](=[O:11])[CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1Participants
6
Procedure
To a solution of the product of Step 1 (15 g) and 50 mL of i-Pr2NEt in 250 mL of CH2Cl2 cooled at 0° C. was added dropwise a solution of sulfur trioxide pyridine complex (23.8 g) in 100 mL of DMSO. After stirring for 10 min, the reaction mixture was treated with 200 mL H2O and extracted with 200 mL of 1:1 EtOAc/hexane. The extract was dried over MgSO4 and concentrated to give 15 g of the title compound as a yellow oil.
Workup
- extractionextracted with 200 mL of 1:1 EtOAc/hexane
- dry with materialThe extract was dried over MgSO4
- concentrationconcentrated
Sources & evidence
- ORD record
- ord-4b14bef825d34615b513de3b60b018a5
- Source dataset
- uspto-grants-2001_04
- Patent number
- US06222048B1
Reaction notes
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