HuagongsheHuagongshe Chemistry Print Report · For research reference only
[(Z)-[1-amino-2-(8-phenyl-1,4-dioxaspiro[4.5]decan-8-yl)ethylidene]amino] acetate → 2-(8-Phenyl-1,4-dioxa-spiro[4.5]dec-8-yl)acetamidine acetic acid salt
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | [(Z)-[1-amino-2-(8-phenyl-1,4-dioxaspiro[4.5]decan-8-yl)ethylidene]amino] acetate | HCID 90271666 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 2-(8-Phenyl-1,4-dioxa-spiro[4.5]dec-8-yl)acetamidine acetic acid salt | HCID 86725948 | 88.8% |
Reaction Steps
To a stirred solution of (Z)-(1-amino-2-{8-phenyl-1,4-dioxaspiro[4.5]decan-8-yl}ethylidene)amino acetate (267) (1.4 g, 4.21 mmol) in methanol was added Pd—C (10%) under nitrogen atmosphere and the mixture was kept under a hydrogen atmosphere of balloon pressure at room temperature for 2 h (reaction was monitored by LC-MS). The reaction mixture was filtered and the filtrate was concentrated in vacuo to get a sticky mass which was triturated with diethyl ether to get pure 2-(8-phenyl-1,4-dioxa-spiro[4.5]dec-8-yl)acetamidine acetic acid salt (268) (1.25 g, 88.79%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09045486B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-a0eecf92da494256998647ea0a9416c2 |
| Source note | uspto-grants-2015_06 |