Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | 4-(2-Oxo-2,3-dihydro-1H-benzimidazol-1-yl)butanoic acid | HCID 13251784 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66603388 | HCID 66603388 | — |
Reaction Steps
Dichloromethane (3772 L) and then 4-(2-oxo-2,3-dihydrobenzimidazol-1-yl)butyric acid (525 kg; 2.4 kmol) were charged to a stirred-tank reactor, followed by N,N-dimethylformamide (21 L). The resulting mixture was cooled to 10° C. Afterward, oxalyl chloride (326.8 kg)) was dosed at 10-15° C. over 2-3 hours while stirring. The resulting mixture was then stirred at 15-20° C. for an additional 1-3 hours. All the above steps were conducted under a N2 atmosphere. Conversion was checked by in-process control (“IPC”).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08362006B2 |
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| Source dataset | uspto-grants-2013_01 |
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| ORD ID | ord-8d957a917e5640ee80e9c395a062742f |
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| Source note | uspto-grants-2013_01 |
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