HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 69108764, compound → HCID 69113200, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 69108764 | HCID 69108764 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 69113200 | HCID 69113200 | 94.5% |
Reaction Steps
Raney nickel 2800 (4.0 g) was added to a degassed solution of the unsaturated ester 43 (4.1 g) in MeOH (150 mL) and the resulting suspension was treated with hydrogen at atmospheric pressure for 18 h. The suspension was filtered over a Celite® bed and concentrated. Flash chromatography (30-50% ethyl acetate in hexane containing 1% acetic acid) of the resulting residue gave the desired saturated ester 44 (3.8 g, 94.5%). 1H NMR (400 MHz, DMSO-d6): 7.54 (d, J=7.6 Hz, 4H), 7.31 (overlapped d, J=8.8 Hz, 2H), 7.29 (overlapped d, J=8.4 Hz, 2H), 4.12 (m, 1H), 3.58 (s, 3H), 2.87 (t, J=7.6 Hz, 2H), 2.65 (t, J 7.6 Hz, 2H), 1.31 (s, 9H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07399786B2 |
| Source dataset | uspto-grants-2008_07 |
| ORD ID | ord-577ca1f72a444a3985afb535bbdd5c32 |
| Source note | uspto-grants-2008_07 |