Sulfuric Acid → HCID 19428701, compound
Reaction equation
[C:1]([S:5][CH2:6][C:7]([OH:17])([CH3:16])[P:8]([O:13][CH2:14][CH3:15])(=[O:12])[O:9][CH2:10][CH3:11])([CH3:4])([CH3:3])[CH3:2].S(=O)(=O)(O)O.ClCCl.[C:26](OC(=O)C)(=[O:28])[CH3:27]>>[C:26]([O:17][C:7]([CH3:16])([P:8]([O:9][CH2:10][CH3:11])(=[O:12])[O:13][CH2:14][CH3:15])[CH2:6][S:5][C:1]([CH3:4])([CH3:2])[CH3:3])(=[O:28])[CH3:27]Participants
5
Conditions
- Temperature
- 20 °C
Procedure
25.2 g (88.6 mmol) of diethyl 2-t-butylthio-1-hydroxy-1-methylethanephosphonate in 130 ml of acetic anhydride are treated with 1 ml of concentrated sulfuric acid, during which process the temperature of the solution rises from 20 to about 30° C. The mixture is subsequently stirred for 8 hours at 20° C., treated with 100 ml of dichloromethane and poured onto 300 ml of ice/water. The organic phase which is separated off is washed in succession with dilute hydrochloric acid, sodium hydrogen carbonate solution and water and dried over sodium sulfate, and the solvent is distilled off in vacuo.
Workup
- customrises from 20 to about 30° C
- customThe organic phase which is separated off
- washis washed in succession with dilute hydrochloric acid, sodium hydrogen carbonate solution and water
- dry with materialdried over sodium sulfate
- distillationthe solvent is distilled off in vacuo
Sources & evidence
- ORD record
- ord-a12f56eb1ace4e9a8e3d772ef86e3a91
- Source dataset
- uspto-grants-1996_08
- Patent number
- US05550276
Reaction notes
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