Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Trityl chloride | HCID 6456 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | (3R)-3-Aminoazepan-2-one--hydrogen chloride (1/1) | HCID 51358597 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 21311272 | HCID 21311272 | 74.5% |
Reaction Steps
To a stirred suspension of 173 g of (R)-α-amino-ε-caprolactam hydrochloride, 266 g of triethylamine and 1,700 ml of chloroform, 293 g of chlorotriphenylmethane was added portionwise under ice-cooling. The resulting mixture was stirred for an hour under the same conditions, and then for two hours at room temperature. The reaction mixture was washed with water and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and to the resultant oily residue 600 ml of n-hexane-ethyl acetate (2:1) mixture was added under heating and stirring. The crystalline precipitates obtained were collected by filtration, washed with 1,000 ml of n-hexane-ethyl acetate (10:1) mixture and dried to provide 290 g of (R)-α-triphenylmethylamino-ε-caprolactam, m.p. 189° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05932568 |
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| Source dataset | uspto-grants-1999_08 |
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| ORD ID | ord-50de8f9c372a4f72a0f6b12d08ff6675 |
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| Source note | uspto-grants-1999_08 |
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