Lawesson's reagent → HCID 22320023, compound
Reaction equation
[CH:1]([C:3]12[CH2:13][CH:8]3[CH2:9][CH:10]([CH2:12][CH:5]([O:6][C:7]3=O)[CH2:4]1)[CH2:11]2)=[CH2:2].COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:24]2)=CC=1>C1(C)C=CC=CC=1>[CH:1]([C:3]12[CH2:13][CH:8]3[CH2:9][CH:10]([CH2:12][CH:5]([O:6][C:7]3=[S:24])[CH2:4]1)[CH2:11]2)=[CH2:2]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 110 °C
Procedure
To a mixture of 6-vinyl-3-oxatricyclo[4.3.1.14,8]undecan-2-one (10 mmol) obtained by the procedure of Example 3 and toluene (50 ml) was added 2,4-bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane 2,4-disulfide [(p-MeO-C6H4P(═S)—S—)2)] (10 mmol), and the resulting mixture was stirred at 110° C. for 24 hours. The reaction mixture was concentrated, the concentrate was subjected to silica gel column chromatography and thereby yielded the title compound 6-vinyl-3-oxatricyclo[4.3.1.14,8]undecane-2-thione in a yield of 75%.
Workup
- concentrationThe reaction mixture was concentrated
Sources & evidence
- ORD record
- ord-8cd5cf4d276b45b68a77ff64a83791f8
- Source dataset
- uspto-grants-2005_09
- Patent number
- US06949615B2
Reaction notes
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