Methanol → HCID 21518711, compound

HRID 1282964Notes

Reaction equation

HRID 1282964 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

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

  1. additionAfter it was poured shallowly into the vessel
  2. 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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