Allylamine → HCID 178456990, compound

HRID 481968

Reaction equation

HRID 481968 reaction equation
O.CS[C:4]1[NH:9][C:8]2[CH:10]=[CH:11][N:12]=[CH:13][C:7]=2[S:6](=[O:15])(=[O:14])[N:5]=1.[CH2:16]([NH2:19])[CH:17]=[CH2:18]>>[CH2:16]([NH:19][C:4]1[NH:9][C:8]2[CH:10]=[CH:11][N:12]=[CH:13][C:7]=2[S:6](=[O:15])(=[O:14])[N:5]=1)[CH:17]=[CH2:18]

Participants

3

Conditions

Temperature
120 °C

Procedure

A mixture of 3-methylsulfanyl-4H-pyrido[4,3-e]-1,2,4-thiadiazine 1,1-dioxide monohydrate (0.5 g) and allylamine (4 mL) was heated in a sealed bumb for 4-5 h at 120° C. After cooling, the amine was removed by distillation under reduced pressure. The residue was dissolved in 0.5N NaOH, treated with charcoal, filtered, and the filtrate was adjusted to pH 6 with 1N HCl. The resulting precipitate was collected by filtration, washed with water and dried to give the title compound as a dihydrate (yield: 0.44 g); m.p. 206°-208° C. (Compound 15).

Workup

  1. temperatureAfter cooling
  2. customthe amine was removed by distillation under reduced pressure
  3. dissolutionThe residue was dissolved in 0.5N NaOH
  4. additiontreated with charcoal
  5. filtrationfiltered
  6. filtrationThe resulting precipitate was collected by filtration
  7. washwashed with water
  8. customdried

Sources & evidence

ORD record
ord-085a166e785e4f3b85065ec9ad85c7db
Source dataset
uspto-grants-1998_08
Patent number
US05792764

Linked notes

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