Dimethylformamide dimethyl acetal → HCID 23565031, compound

HRID 1059454Notes

Reaction equation

HRID 1059454 reaction equation
[NH2:1][CH2:2][C:3]1[CH:4]=[CH:5][C:6]2[S:11][C:10]3[N:12]=[CH:13][CH:14]=[N:15][C:9]=3[NH:8][C:7]=2[CH:16]=1.CO[CH:19](OC)[N:20]([CH3:22])[CH3:21]>O1CCCC1.CO>[CH3:19][N:20]([CH3:22])[CH:21]=[N:1][CH2:2][C:3]1[CH:4]=[CH:5][C:6]2[S:11][C:10]3[N:12]=[CH:13][CH:14]=[N:15][C:9]=3[NH:8][C:7]=2[CH:16]=1

Participants

5

Reactant 2

HCID 78373Dimethylformamide dimethyl acetalHCID 18670209HCID 18670209, compound

Product 1

HCID 23565031HCID 23565031, compoundYield 80.7%

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 8028TetrahydrofuranSolvent

Conditions

Temperature
40 °C

Procedure

400 mg of 8-(aminomethyl)-10H-pyrazino[2,3-b][1,4]benzothiazine was dissolved in tetrahydrofuran (5 ml)/methanol (5 ml). After adding 250 mg of N,N-dimethylformamide dimethyl acetal, the resulting mixture was heated to 40° C. for 1.5 hours. After distilling off the solvent under reduced pressure, the crystals thus precipitated were taken up by filtration and washed successively with diethyl ether and diisopropyl ether. Thus 400 mg of the title compound was obtained as yellow crystals.

Workup

  1. distillationAfter distilling off the solvent under reduced pressure
  2. customthe crystals thus precipitated
  3. filtrationwere taken up by filtration
  4. washwashed successively with diethyl ether and diisopropyl ether

Sources & evidence

ORD record
ord-d036e05f72844ac2a305bab08f505bc2
Source dataset
uspto-grants-2003_02
Patent number
US06518423B1

Reaction notes

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