Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Delta-Valerolactone | HCID 10953 | — |
| Reactant | N-Methylhydrazinecarbothioamide | HCID 2723853 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 57691901 | HCID 57691901 | — |
Reaction Steps
Tetrahydro-2H-pyran-2-one (2 ml), N-methylhydrazinecarbothioamide (3.4 g) and acetic acid (0.3 ml) were suspended in methanol (10 ml). The reaction was heated in microwave oven at 120° C. for 20′ followed by further 10′ at 110° C. Acetic acid was added (0.3 ml) and reaction was heated in a microwave oven at 140° C. for 20′, further acetic acid (0.3 ml) was added and the reaction was in a microwave oven at 140° C. for 20′. The solvent was removed under reduced pressure, DCM was added to the crude and solid filtered-off. Solvent was removed under reduced pressure to give a crude product that was purified by flash chromatography on silica gel (DCM/MeOH from 0 to 10%) to give the title compound as a white solid (1 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07947683B2 |
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| Source dataset | uspto-grants-2011_05 |
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| ORD ID | ord-266297101bcb4ecebaa586908cb50183 |
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| Source note | uspto-grants-2011_05 |
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