HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetonitrile → HCID 58168476, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | tert-Butyl acrylate | HCID 15458 | — |
| Reactant | Benzyltrimethylammonium hydroxide | HCID 66854 | — |
| Reactant | HCID 58168599 | HCID 58168599 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 58168476 | HCID 58168476 | — |
Reaction Steps
Benzyltrimethylammonium hydroxide (40% in water, 0.27 mL) was added in one portion to a stirred solution of (9-(2-(5-(2-hydroxyethyl)thiophen-3-yl)ethyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)(2-isopropylthiazol-4-yl)methanone [Example 78, step b] (0.92 g) and tert-butyl acrylate (0.38 g) in toluene (1 mL). The resultant mixture was stirred vigorously at 20° C. for 4 hours. Acetonitrile (1 mL) was added and the mixture was stirred for 18 hours and then purified without work up. The crude product was purified by flash silica chromatography, using 6% methanol in ethyl acetate with 1% triethylamine as solvent. Fractions containing the product were evaporated to dryness to afford the subtitled compound. Yield 0.84 g.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08476265B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-60631ba96e5d4f28a6096fd22dfc1025 |
| Source note | uspto-grants-2013_07 |