HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 86623587, compound → HCID 68852899, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 86623587 | HCID 86623587 | — |
| Reactant | HCID 178418573 | HCID 178418573 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 68852899 | HCID 68852899 | 61.2% |
Reaction Steps
9b (1.7 g, 6.5×10−3 mol) in diethyl ether (50 ml) was added dropwise at 10° C. to a solution of methylmagnesium bromide (3 ml of 3M diethyl ether solution, 9.0×10−3 mol) in the same solvent (50 ml). The reaction mixture was stirred at r. t. for additional 2 h, poured into ice-cold 0.1M HCl (100 ml) and extracted with MTBE (100 ml). The organic phase was washed with brine (2×50 ml), dried (MgSO4), concentrated in vacuo and purified by recrystallisation from hexane to afford 3-(2,2,7,7-tetramethyltricyclo[6.2.1.01,6]undec-5-en-5y-1)butan-2-ol (10b, 1.1 g, 61% yield, white prisms, m.p. 119-121° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07550417B2 |
| Source dataset | uspto-grants-2009_06 |
| ORD ID | ord-0c152ebd13684cc58c0919d645330a71 |
| Source note | uspto-grants-2009_06 |