HuagongsheHuagongshe Chemistry Print Report · For research reference only
TBAF tetrahydrofuran → HCID 178484178, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | TBAF tetrahydrofuran | HCID 11078149 | — |
| Reactant | HCID 178484179 | HCID 178484179 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178484178 | HCID 178484178 | 64% |
Reaction Steps
tert-Butyl (S)-1-(trans-4-(t-butyldimethylsilyloxy)cyclohexyl)-3-(N-(benzyloxycarbonyl)-N-methylamino)propan-2-ylcarbamate (18 g, 34 mmol) was treated with 4 M nBu4NF/THF (50 mL) at 50° C. for 6 h. Water (30 mL) was added and the mixture was extracted with EtOAc (3×100 mL). The combined organic layers were washed with brine, dried over MgSO4 and evaporated to give crude tert-butyl (S)-1-(trans-4-hydroxycyclohexyl)-3-(N-(benzyloxycarbonyl)-N-methylamino)propan-2-ylcarbamate (9 g, 64%) that was purified by silica chromatography. 1H NMR (CDCl3, 400 MHz) δ 1.41 (d, 9H), 1.65 (m, 6H), 1.95 (m, 3H), 2.98 (d, 3H), 3.10 (m, 1H), 3.52 (m, 1H), 3.90 (m, 1H), 5.13 (d, 2H), 7.33 (m, 5H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08487108B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-dd31fa7b67e4489db893784bf53fda56 |
| Source note | uspto-grants-2013_07 |