Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | Dibah | HCID 16682954 | — |
| Reactant | HCID 22481040 | HCID 22481040 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 22481030 | HCID 22481030 | 76.9% |
Reaction Steps
280 mg (0.52 mmol) of the compound from Example 4 are dissolved in 40 ml of abs. toluene and, at from −10° C. to −15° C., admixed dropwise with 3.5 ml of 25% strength diisobutylaluminium hyride solution. The mixture is stirred for 1 hour, cooled to −70° C. and admixed dropwise with 0.2 ml of methanol. At 20° C., the mixture is admixed with sodium chloride solution, the phases are separated and the organic phase is dried. The evaporation residue is purified over a silica gel column Crystallization from heptane gives 195 mg of colourless crystals of m.p. 126-127° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06562976B2 |
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| Source dataset | uspto-grants-2003_05 |
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| ORD ID | ord-99675d1ee4d44401a93e890f709f64fa |
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| Source note | uspto-grants-2003_05 |
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