Magnesium → HCID 19697802, compound

HRID 863276Notes

Reaction equation

HRID 863276 reaction equation
[CH2:1]([O:3][C:4]([CH:6]1[NH:11][C:10]2[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=2[O:8][CH2:7]1)=[O:5])C.[Mg]>CO>[CH3:1][O:3][C:4]([CH:6]1[NH:11][C:10]2[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=2[O:8][CH2:7]1)=[O:5]

Participants

4

Reactant 2

HCID 5462224MagnesiumHCID 10703520HCID 10703520, compound

Product 1

HCID 19697802HCID 19697802, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

4.0 g of 3(R,S)-ethoxycarbonyl-3,4-dihydro-2H-1,4-benzoxazine (Example 20)) are stirred together with 0.8 g of magnesium powder in 100 ml of methanol at room temperature for 2 h. When the exothermic reaction has ended, the mixture is concentrated, the residue is taken up in methylene chloride and the organic phase is washed with 0.1N hydrochloric acid. After customary working up, the crude product is purified over 250 g of silica gel (mobile phase B): Rf (B)=0.26.

Workup

  1. customWhen the exothermic reaction
  2. concentrationthe mixture is concentrated
  3. washthe organic phase is washed with 0.1N hydrochloric acid
  4. customthe crude product is purified over 250 g of silica gel (mobile phase B)

Sources & evidence

ORD record
ord-def8c20d37c44b9a9947156f08442db5
Source dataset
uspto-grants-1998_02
Patent number
US05719141

Reaction notes

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