HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 71060138, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 4-(Chlorosulfonyl)benzoic acid | HCID 82385 | — |
| Reactant | 4-(N-Boc-amino)piperidine | HCID 723833 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 71060138 | HCID 71060138 | 119.7% |
Reaction Steps
Diisopropylethylamine (10.9 ml, 62.4 mmol) was added in one portion to a stirred solution of piperidin-4-yl-carbamic acid tert-butyl ester (5.0 g, 20.0 mmol) in THF (150 ml) at room temperature. To this mixture was added 4-(chlorosulfonyl)benzoic acid (5.52 g, 25.0 mmol) portion wise and the mixture was stirred at room temperature under a nitrogen atmosphere for 1 hour. After this time the mixture was concentrated and the resulting residue suspended in HCl (1M solution, 100 ml), the resulting solid precipitate was collected by filtration, washed with water and dried under vacuum give the title compound (9.2 g, 96% yield) as a white solid. Tr=1.28 min m/z (ES+) (M+Na+) 407.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08889716B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-135e1ff799c247f6bc20ce394b02e2da |
| Source note | uspto-grants-2014_11 |