Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | 2-Ethylbutanedioyl dichloride | HCID 21864608 | — |
| Reactant | HCID 23031791 | HCID 23031791 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 54752976 | HCID 54752976 | 76.7% |
Reaction Steps
DBU (211 ml) was added to a solution of (3-bromophenyl) (4-chloro-2-hydroxy-5-methylphenyl)methanone (170 g) in acetonitrile (510 ml) at 25 to 30° C. Then, a solution of ethyl succinic chloride (146 g) in acetonitrile (340 ml) was added dropwise over 30 minutes at 25 to 40° C. After the drop was completed, the mixture was stirred at 30° C. for 1 hour. Water (94 ml) was added dropwise keeping the reaction solution at 25 to 30° C. After the mixture was stirred at the same temperature for 1 hour, the resulting crystals were filtered, and washed with a mixture of acetonitrile and water (9/1, 170 ml) four times, dried under reduced pressure to obtain the title compound (174 g, yield 76.7%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07541478B2 |
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| Source dataset | uspto-grants-2009_06 |
|---|
| ORD ID | ord-3e8f19f522cd4c56b4b8ec5deeab5cb2 |
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| Source note | uspto-grants-2009_06 |
|---|