HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 59733746, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 68977302 | HCID 68977302 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 59733746 | HCID 59733746 | — |
Reaction Steps
A solution of 8-(3-tert-Butyl-phenyl)-1,4-dioxa-spiro[4.5]dec-8-ylamine hydrochloride (337 mg, 1.03 mmol) in glacial acetic acid (9 mL) and water (4 mL) was heated to 75° C. for 21 h, whereupon the reaction was deemed complete by HPLC analysis. The reaction mixture was basified with 2.5 N NaOH solution, then extracted with ethyl acetate (3×25 mL). The combined organic layers were washed (brine), dried (Na2SO4), filtered and concentrated under reduced pressure. Material was pure by HPLC/MS: retention time=1.18 min, method [7]; mass spec (ESI) 246 (MH+, 33), 229 (M−NH2+, 100), 228 (28), 173 (47).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07385085B2 |
| Source dataset | uspto-grants-2008_06 |
| ORD ID | ord-f47a763c48f34693ae19a479f2c6378d |
| Source note | uspto-grants-2008_06 |