Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Acetoxyacetyl chloride | HCID 26297 | — |
| Reactant | HCID 68701920 | HCID 68701920 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59161011 | HCID 59161011 | — |
Reaction Steps
5 g of the crude product from Example 20A are suspended in 24 ml of dichloromethane and cooled to 0° C. 1.88 g (13.79 mmol) of acetoxyacetyl chloride and 5.9 ml (42.42 mmol) of triethylamine are added. The reaction mixture is stirred at RT for 8 h. After addition of 25 ml of dichloromethane the mixture is washed once with 10 ml of water and once with 10 ml of saturated aqueous sodium chloride solution. The organic phase is dried over magnesium sulfate. After removal of the solvent on a rotary evaporator the residue is purified chromatographically on silica gel 60 (mobile phase: gradient cyclohexane/ethyl acetate 20:1→1:1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08304412B2 |
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| Source dataset | uspto-grants-2012_11 |
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| ORD ID | ord-7c2f2eb20d1e49c48d9b964afb7071e4 |
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| Source note | uspto-grants-2012_11 |
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