HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 22327806, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 6-Methyl-6-isobutylfulvene | HCID 562618 | — |
| Reactant | HCID 178418348 | HCID 178418348 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 22327806 | HCID 22327806 | 80% |
Reaction Steps
To a solution of 8.00 g (54.0 mmol) of 6-methyl-6-isobutylfulvene in 30 ml of ether, 54.0 ml (61.6 mmol) of an ether solution of methyllithium was dropwise added in a nitrogen atmosphere with ice cooling, followed by stirring at room temperature for 4 days. Then, 30 ml of water was added. The separated organic phase was washed with water and a saturated saline solution, then dried over magnesium sulfate and filtered. From the filtrate, the solvent was removed under reduced pressure to obtain a liquid. The liquid was subjected to vacuum distillation (120° C./25 mmHg) to obtain 7.10 g (43.2 mmol) of a light yellow liquid (yield: 80%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07449533B2 |
| Source dataset | uspto-grants-2008_11 |
| ORD ID | ord-911eee3c27904bc59bc847f14493b0c2 |
| Source note | uspto-grants-2008_11 |