Chloroform → HCID 131718303, compound
Reaction equation
[Br:1][CH2:2][C:3]([CH:5]1[CH:10]2[CH:8]([C:9]2([CH3:12])[CH3:11])[C:7](=[O:13])[O:6]1)=[O:4].C(Cl)Cl.C(Cl)(Cl)Cl.[Br:21]Br>O>[Br:1][CH:2]([Br:21])[C:3]([CH:5]1[CH:10]2[CH:8]([C:9]2([CH3:11])[CH3:12])[C:7](=[O:13])[O:6]1)=[O:4]Participants
6
Reactant 4
Product 1
Reagents, catalysts & solvents 1
Procedure
0.125 g of (1R-(1 α, 4 β, 5α))-4-(bromoacetyl)-6,6-dimethyl-3-oxabicyclo [3.1.0] hexan-2-one of Example 3 were mixed under an inert ga atmosphere with 1 ml of methylene chloride and 1 ml of chloroform. 50 μl of bromine were added slowly at +25° to 30° C. and the mixture was stirred for 48 hours at ambient temperature. Water was added, followed by decanting and extracting with methylene chloride. The organic phase was dried and the solvent was evaporated under reduced pressure to obtain 0.199 g of the crude expected product in the form of an oil.
Workup
- customby decanting
- extractionextracting with methylene chloride
- customThe organic phase was dried
- customthe solvent was evaporated under reduced pressure
Sources & evidence
- ORD record
- ord-74d36dc664534f3a8ed612eee48ff4cc
- Source dataset
- uspto-grants-1994_01
- Patent number
- US05276167
Reaction notes
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