Hydrogen chloride-ethyl acetate → HCID 66881276, compound
Reaction equation
[Br:1][C:2]1[CH:3]=[C:4]([NH:11]C(=O)OC(C)(C)C)[C:5]2[O:9][CH2:8][CH2:7][C:6]=2[CH:10]=1.[ClH:19].C(OCC)(=O)C>C(OCC)(=O)C>[ClH:19].[Br:1][C:2]1[CH:3]=[C:4]([NH2:11])[C:5]2[O:9][CH2:8][CH2:7][C:6]=2[CH:10]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
The compound (6.27 g, 20.0 mmol) obtained in step A was dissolved in ethyl acetate, 4N hydrochloric acid-ethyl acetate solution (25 ml, 100 mmol) was added at room temperature with stirring, and the mixture was stirred at the same temperature overnight. The precipitated solid was filtered, washed with ethyl acetate, and dried under reduced pressure to give the title compound (4.65 g, yield 93%) as a colorless solid.
Workup
- stirringthe mixture was stirred at the same temperature overnight
- filtrationThe precipitated solid was filtered
- washwashed with ethyl acetate
- customdried under reduced pressure
Sources & evidence
- ORD record
- ord-bd3bedd2808c48d599b9de5c7b2ec225
- Source dataset
- uspto-grants-2013_08
- Patent number
- US08513235B2
Reaction notes
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