HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorodichloridic acid, phenyl ester → HCID 66687284, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorodichloridic acid, phenyl ester | HCID 13038 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Methyl 2-aminoisobutyrate hydrochloride | HCID 13258034 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66687284 | HCID 66687284 | — |
Reaction Steps
A solution of phenylphosphorodichloridate (1.0 eq., 13.0 mmol, 1.9 mL) and methyl α-aminoisobutyrate hydrochloride (1.0 eq., 13.0 mmol, 2.0 g) in CH2Cl2 (80 mL) was cooled to −80° C. Dry N,N-diisopropylethylamine (DIPEA; 2.0 eq., 26.0 mmol, 4.3 mL) was added dropwise. After 2 hours, the reaction was warmed to room temperature and the solvent was removed under reduced pressure. Dry diethylether was added and the precipitate was filtered off and washed twice with dry diethylether under an argon atmosphere. The filtrate was evaporated to dryness to give 11 which was stored as a 0.90 M solution in dry tetrahydrofuran (THF) at −18° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08481510B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-f343df31c4eb4d41a41b36c4399ebc54 |
| Source note | uspto-grants-2013_07 |