HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 178457232, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 4-Chlorophenyl chloroformate | HCID 139059 | — |
| Reactant | HCID 178457231 | HCID 178457231 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Solvent | Ether sodium bicarbonate | HCID 23682952 | — |
| Product | HCID 178457232 | HCID 178457232 | 67.2% |
Reaction Steps
A solution of 66 mg (0.3 mmol) of trans-{4-[3-(Allyl-methyl-amino)-prop-1-ynyl]-cyclohexyl}-methyl-amine in 0.3 ml dioxane was treated with 0.103 ml (0.6 mmol; 2 equivalents) Huenig's base and dropwise with a solution of 0.042 ml (0.27 mmol) 4-chlorophenylchloroformate in 0.16 ml dioxane (during 10 min). After 5 min at RT, the mixture was dissolved in aqueous saturated NaHCO3/Et2O (3×). The organic phase was dried over Na2SO4 and evaporated. Flash column chromatography on silica gel with CH2Cl2/MeOH (99:1 to 97:3) yielded 68 mg (61%) of trans-{4-[3-(Allyl-methyl-amino)-prop-1-ynyl]-cyclohexyl}-methyl-carbamic acid 4-chloro-phenyl ester, MS: 375 (MH+, 1Cl).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06858651B2 |
| Source dataset | uspto-grants-2005_02 |
| ORD ID | ord-e00da6cf44d6447186086da1eba9ec4a |
| Source note | uspto-grants-2005_02 |