Methanol → HCID 21518711, compound
Reaction equation
[CH2:1]([O:4][NH:5][C:6](=[C:9]1[C:14](=[O:15])[CH:13]=[C:12]([CH2:16][CH3:17])[O:11][C:10]1=[O:18])[CH2:7][CH3:8])[CH:2]=[CH2:3].C[OH:20]>CC(C)=O.O>[CH2:1]([O:4][NH:5][C:6]([CH:9]1[C:14](=[O:15])[CH:13]=[C:12]([CH2:16][CH3:17])[O:11][C:10]1=[O:18])([OH:20])[CH2:7][CH3:8])[CH:2]=[CH2:3]Participants
5
Reactant 2
Product 1
Reagents, catalysts & solvents 2
Procedure
1.0 g of 3-(1-allyloxyaminopropylidene)-6-ethyl-3,4-dihydro-2H-pyrane-2,4-dione (ND26.5 :1.5389) was dissolved in 50ml of acetone containing 5% of water. After it was poured shallowly into the vessel having an area of (30×35)cm2, it was allowed to stand for a day in the sunlight. 630mg of the crude product was obtained by the distillation of methanol after the precipitated crystal on the container was recovered by washing with methanol. The crude product was recrystallized three times from the mixture of ethanol and water and 300mg of 3-(1-allyloxyamino-1-hydroxypropyl)-6-ethyl-3,4-dihydro-2H-pyrane-2,4-dione having a melting point of 62.5° to 64°C as a white crystal was obtained.
Workup
- additionAfter it was poured shallowly into the vessel
- waitto stand for a day in the sunlight
Sources & evidence
- ORD record
- ord-6da5948a96be4349bb97f50cfa4068f4
- Source dataset
- uspto-grants-1976_08
- Patent number
- US03973945
Reaction notes
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