HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 59557729, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 1-Bromo-2-butyne | HCID 2756862 | — |
| Reactant | 3-(2-Bromo-5-chloro-4-(4-ethoxybenzyl)phenyl)propan-1-ol | HCID 59557706 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59557729 | HCID 59557729 | 65.6% |
Reaction Steps
To a stirred solution of 3-(2-bromo-5-chloro-4-(4-ethoxybenzyl)phenyl)propan-1-ol (BL) (0.268 g, 0.70 mmol) in 5 mL of THF was added NaH (0.034 g, 0.84 mmol, 60%) and stirred for 40 min. 1-bromo-2-butyne (0.094 mL, 1.05 mmol) was added and the mixture was stirred overnight at room temperature. The reaction was quenched with water and extracted with ethyl acetate. The combined organic layers were washed with water and brine, dried over Na2SO4, concentrated and purified by preparative TLC (eluting with EtOAc:PE=1:10) to obtain 0.2 g of intermediate BM.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07838498B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-754414dff5ca4009b086c461394b7518 |
| Source note | uspto-grants-2010_11 |