HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,3-DI-Boc-2-methylisothiourea → HCID 178454258, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,3-DI-Boc-2-methylisothiourea | HCID 546603 | — |
| Reactant | BIS(8-AMINOOCTYL)AMINE | HCID 10199351 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | MeOH tetrahydrofuran | HCID 21899815 | — |
| Product | HCID 178454258 | HCID 178454258 | — |
Reaction Steps
To a stirred solution of 1,17-diamino-9-azaheptadecane 3 (4.9 g, 15.06 mmol) in THF/CH3OH 5/3 (80 mL) at 50° C., a solution of N,N′-bis(tert-butoxycarbonyl)-S-methylisothiourea (1.456 g, 5.02 mmol) in THF (25 mL) was added dropwise over 1 h. After 16 h, the reaction mixture was concentrated under reduced pressure and the residue was purified by flash chromatography (6% methanol, 4% triethylamine, 90% ethyl acetate), affording 12 as a pale yellow oil, 3.51 g (70%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08685953B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-50f7af91c1e24a149147b554c3192051 |
| Source note | uspto-grants-2014_04 |