Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Methane, dichloromethoxy- | HCID 21004 | — |
| Reactant | HCID 25006074 | HCID 25006074 | — |
| Catalyst | Titanium Tetrachloride | HCID 24193 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 25003272 | HCID 25003272 | 77% |
Reaction Steps
1.0M Titanium tetrachloride in dichloromethane solution (2 mL, 2.0 mmol) was added to a suspension of 2-aminocarbonylamino-5-(3-chlorophenyl)pyrrole-3-carboxamide (Compound No. 1-25, 140 mg, 0.50 mmol) in dichloromethane (3 mL) at −30° C. and the mixture was stirred for 40 minutes. Moreover, dichloromethyl methyl ether (0.27 mL, 3.0 mmol) was added thereto and the whole was stirred overnight at 4° C. Under ice-cooling, 1N hydrochloric acid (4 mL) was added thereto and the mixture was stirred for 1 hour, and then water (10 mL) was add thereto. The precipitated solid was filtered off, washed with chloroform (10 mL) and water (10 mL), and dried under reduced pressure to give the target compound (120 mg) as a brown solid (Yield 77%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07977371B2 |
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| Source dataset | uspto-grants-2011_07 |
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| ORD ID | ord-3ff38c842c8342218af6d7100fb8de1e |
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| Source note | uspto-grants-2011_07 |
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