Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetone | HCID 180 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2-Bromo-6-benzoylthioureidopyridine | HCID 20635540 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | (6-Bromo-pyridin-2-YL)thiourea | HCID 22170428 | — |
Reaction Steps
4.933 g (14.67 mmol) N-{[(6-bromopyridin-2-yl)amino]carbonothioyl}benzamide was suspended in 40 mL methanol and additionally combined with 7 mL acetone. After addition of 1 N sodium hydroxide solution (40.0 mmol) the reaction mixture became completely clear with a light brown color. The mixture was heated for 40 min at 65° C. (oil bath temperature) and then stirred for 1 hr at room temperature. A solid crystallized out. The organic solvent was removed under vacuum, and after cooling on an ice bath the solid was filtered off and washed with water. The solid was dried over phosphorus pentoxide in a dessicator under high vacuum (4×10 mbar). The desired product N-(6-bromopyridin-2-yl)thiourea was obtained in the form of colorless needles in a yield of 3.158 g (13.61 mmol, 93%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09296697B2 |
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| Source dataset | uspto-grants-2016_03 |
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| ORD ID | ord-453275f6e3824467b76a85920ac3bcba |
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| Source note | uspto-grants-2016_03 |
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