2-Aminopropanol → HCID 178460116, compound

HRID 481970

Reaction equation

HRID 481970 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.[NH2:16][CH:17]([CH3:20])[CH2:18][OH:19]>C(OCC)C>[OH:19][CH2:18][CH:17]([NH:16][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)[CH3:20]

Participants

4

Reactant 2

HCID 51262-AminopropanolHCID 190647513-Methylsulfanyl-4H-pyrido[4,3-e]-1,2,4-thiadiazine 1,1-dioxide monohydrate

Product 1

HCID 178460116HCID 178460116, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

A suspension of 3-methylsulfanyl-4H-pyrido[4,3-e]-1,2,4-thiadiazine 1,1-dioxide monohydrate and 2-amino-1-propanol (0.75 mL) was refluxed for 90 min (until completion of the reaction; t.l.c.). After cooling, the addition of diethylether (20 mL) gave rise to the separation of an oily residue. After decantation of the etheral solution, the residue was solubilized in methanol (1 mL) and then supplemented with diethylether (15 mL). An oily residue separated again. After decantation of the supernatent, the oily residue was solubilized in acetone (6 mL). A fine precipitate readily appeared. After 3 h at +4° C., the resulting precipitate was collected by filtration, washed with acetone and dried (yield: 0.33 g); m.p. 213°-216° C. (Compound 19).

Workup

  1. temperaturewas refluxed for 90 min (
  2. customuntil completion of the reaction
  3. temperatureAfter cooling
  4. customgave rise
  5. customto the separation of an oily residue
  6. customAn oily residue separated again
  7. filtrationthe resulting precipitate was collected by filtration
  8. washwashed with acetone
  9. customdried (yield: 0.33 g)

Sources & evidence

ORD record
ord-c0c6d6652c6e44438236c643e2c99a69
Source dataset
uspto-grants-1998_08
Patent number
US05792764

Linked notes

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