Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 1-Butanol | HCID 263 | — |
| Reactant | Cyanamide | HCID 9864 | — |
| Reactant | HCID 86587667 | HCID 86587667 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86587668 | HCID 86587668 | — |
Reaction Steps
The mixture of a hydrochloride salt of 1 (285 mg, 0.54 mmol), cyanamide (50 mg, 1.19 mmol) and 1-butanol (2 ml) was stirred at 120° C. for 2 hours. The cooled mixture was diluted with CH2Cl2(50 ml) and washed with saturated aqueous NaCl(Brine)/methanol 1:1 (50 ml). The organic layer was then dried (Na2SO4), evaporated to an oil and chromatographed on a column of silica gel using CH2Cl2/methanol/conc. NH4OH 40:10:2 giving 80 mg of the desired material (yield, 28%). 1H NMR (CDCl3) d 7.08 (br s, 1H, NH), 5.34 (m, 2H, CH═CH), 3.29 (m, 4H), 2.00 (m, 4H), 1.62 (m, 4H), 1.25 (m, 48H), 0.88 (m, 6H). FAB-MS: 535 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07553830B2 |
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| Source dataset | uspto-grants-2009_06 |
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| ORD ID | ord-187f9c4cabef4ef19e9ddc374a688426 |
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| Source note | uspto-grants-2009_06 |
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