Hydrogen chloride-ethyl acetate → HCID 67519776, compound
Reaction equation
[ClH:1].C(OCC)(=O)C.C(OC([NH:15][C:16]1([CH2:22][CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1)=O)(C)(C)C>C(OCC)(=O)C>[ClH:1].[NH2:15][C:16]1([CH2:22][CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH2:17][CH2:18][O:19][CH2:20][CH2:21]1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
4N hydrochloric acid-ethyl acetate solution (12.9 mL, 51.6 mmol) was added in a ethyl acetate (40 mL) solution of ethyl 3-(4-t-butoxycarbonylamino-tetrahydro-pyran-4-yl)-propionate (2.59 g, 8.6 mmol), which had been obtained in 4), in an ice bath. The reaction mixture was stirred at room temperature for 4 hours, and 4N hydrochloric acid-ethyl acetate solution (4.3 mL, 17.2 mmol) was added and the reaction mixture was further stirred at room temperature for 1 hour. The formed solid was filtered to give a colorless solid (BB05, 1.28 g).
Workup
- customhad been obtained in 4), in an ice bath
- stirringthe reaction mixture was further stirred at room temperature for 1 hour
- filtrationThe formed solid was filtered
- customto give a colorless solid (BB05, 1.28 g)
Sources & evidence
- ORD record
- ord-2837e435d572476d9c1840759e08704f
- Source dataset
- uspto-grants-2013_02
- Patent number
- US08367666B2
Reaction notes
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