HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Decanol → HCID 10356104, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Decanol | HCID 8174 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 6-Chloropurine | HCID 5359277 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 10356104 | HCID 10356104 | 61.3% |
Reaction Steps
1-Decanol (13ml, 68.2mmol) was added in one portion to a stirred suspension of a 60% dispersion of sodium hydride in oil (2.70 g, 67.5mmol) in dry tetrahydrofuran (70 ml) under an atmosphere of nitrogen. Gas was evolved. After 0.5 h 6-chloropurine (3.00 g, 19.4 mmol) was added and the suspension heated at reflux for 3.5 h. The tetrahydrofuran was removed in vacuo and the residue suspended in dilute hydrochloric acid (200 ml). The acidic suspension was stirred for 1 h then neutralised with saturated sodium hydrogen carbonate solution. The suspension was stirred vigorously with 60-80 petroleum ether (500 ml) and the solid removed by filtration. The solid was recrystallised from methanol to give a white solid (3.29 g, 11.9 mmol, 61%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06309811B2 |
| Source dataset | uspto-grants-2001_10 |
| ORD ID | ord-6937d6ebafde4a0393d0ca0ef60b5956 |
| Source note | uspto-grants-2001_10 |