Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Guanidine Hydrochloride | HCID 5742 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Benzyl chloroformate | HCID 10387 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Solvent | Water | HCID 962 | — |
| Product | 10065-79-9 | HCID 137832551 | — |
Reaction Steps
A 100 L glass lined reactor equipped with a mechanical agitator, cooling jacket, condenser, and addition lines was charged with THF (15.53 kg) and guanidine HCl (3.10 kg, 32.02 mol). To the resultant slurry was added purified water (5.00 kg) and 50% sodium hydroxide solution (8.61 kg, 100.75 mol). The resultant slurry was cooled to 4-6° C. and benzyl chloroformate (13.02 kg, 72.51 mol) was slowly added over a 3.5-hour period, while keeping the temperature below 10° C. The resultant slurry was stirred for 2 hours at a temperature between 5-10° C. The slurry was then filtered and the solids washed with THF (5.58 kg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08309720B2 |
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| Source dataset | uspto-grants-2012_11 |
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| ORD ID | ord-7276777d1abc43a3a4589e09973760c1 |
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| Source note | uspto-grants-2012_11 |
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