Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Malononitrile | HCID 8010 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 22714268 | HCID 22714268 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22714258 | HCID 22714258 | — |
Reaction Steps
Under argon, 400 mg (10.0 mmol) of sodium hydride (60% suspension in oil) are suspended at room temperature in 40 ml of THF. A solution of 661 mg (10.0 mmol) of malonodinitrile in 10 ml of THF is added dropwise, and the reaction mixture is stirred for 15 min. A solution of 891 mg (5.0 mmol) of 2-methyl-5-methylsulphonyl-1,3,4-thiadiazole in 10 ml of THF is added dropwise. The reaction mixture is heated to 50° C. and stirred overnight, cooled and concentrated using a rotary evaporator. The residue is dissolved in water and adjusted to pH=3 using HCl. A brown solid precipitates out, and this solid is filtered off and dried under reduced pressure.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06743798B1 |
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| Source dataset | uspto-grants-2004_06 |
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| ORD ID | ord-7f150fb4aa00482d854c32916334f859 |
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| Source note | uspto-grants-2004_06 |
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