Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | HCID 19076394 | HCID 19076394 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 19076549 | HCID 19076549 | 56.1% |
Reaction Steps
A solution of 0.034 g of acetyl chloride in 0.5 ml of DCM is added at RT to a solution of 0.276 g of the compound obtained in EXAMPLE 199, in the form of the free base, and 2 ml of pyridine in 2 ml of DCM and the mixture is stirred for 1 hour. A further 0.034 g of acetyl chloride is added and the reaction mixture is stirred for 30 minutes at RT and concentrated under vacuum. The residue is taken up with AcOEt, the organic phase is washed with water and with a saturated solution of NaCl and dried over sodium sulfate and the solvent is evaporated off under vacuum. The residue is chromatographed on silica using a DCM/AcOEt mixture (50/50; v/v) as the eluent to give 0.14 g of the expected product after crystallization from a DCM/iso ether mixture. M.p.=195°-198° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05773612 |
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| Source dataset | uspto-grants-1998_06 |
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| ORD ID | ord-709ff7ec1b1d43a5be261ad1a817e4dd |
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| Source note | uspto-grants-1998_06 |
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