Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 89924015 | HCID 89924015 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 89938248 | HCID 89938248 | 87.6% |
Reaction Steps
To a stirred solution of lithium aluminium hydride (0.774 g, 20.4 mmol) in tetrahudrofuran (20 mL) was added ethyl 2-(4-(4-fluorophenyl)piperazin-1-yl)-2-methylpropanoate (prepared according to procedure reported in Bioorganic & Medical Chemistry, 2006, 14, 2725; 2.0 g, 6.79 mmol) in tetrahudrofuran (10 mL) was added slowly at 25° C. The resulting mixture was then stirred for 16 h. After completion of reaction, ethyl acetate (5 ml) was added followed by 1N Sodium hydroxide (20 ml) and allowed to stirred for 1 h. It was then passed through a celite bed and washed with ethyl acetate (100 ml. To the filtrate water (50 ml) was added and extracted with ethyl acetate (3×50 mL), combined organic layers was dried over sodium sulphate and concentrated to afford crude product. Crude product was purified by using silica gel (100-200 mesh) column chromatography using 5% methanol in dichloromethane as eluent to obtain the titled compound (1.5 g, 87.0%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09359367B2 |
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| Source dataset | uspto-grants-2016_06 |
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| ORD ID | ord-6d759e8b9e3446dabb6126c17b6c90c8 |
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| Source note | uspto-grants-2016_06 |
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