Isopropanol → HCID 18998380, compound

HRID 2260490Notes

Reaction equation

HRID 2260490 reaction equation
[CH3:1][N:2]([CH3:17])[C:3]1[N:16]=[C:6]2[N:7]=[C:8]3[CH2:15][CH2:14][CH2:13][S:12][C:9]3=[C:10](Cl)[N:5]2[N:4]=1.CC(O)C.[NH2:22][CH2:23][CH2:24][N:25]1[CH2:30][CH2:29][O:28][CH2:27][CH2:26]1.Cl.C(N(CC)CC)C>C(N(CC)CC)C>[CH3:1][N:2]([CH3:17])[C:3]1[N:16]=[C:6]2[N:7]=[C:8]3[CH2:15][CH2:14][CH2:13][S:12][C:9]3=[C:10]([NH:22][CH2:23][CH2:24][N:25]3[CH2:30][CH2:29][O:28][CH2:27][CH2:26]3)[N:5]2[N:4]=1

Participants

6

Reactant 4

HCID 3776IsopropanolHCID 11130Triethylamine hydrochlorideHCID 4082852-MorpholinoethylamineHCID 18998329HCID 18998329, compound

Product 1

HCID 18998380HCID 18998380, compound

Reagents, catalysts & solvents 1

HCID 8471TriethylamineSolvent

Procedure

To a suspension of 5.40 g (0.02 mole) of 2-(dimethylamino)-5-chloro-7,8-dihydro-9H-thiopyrano[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidine in 20 ml of 2-propanol 2,125 g (0.021 mole) of triethylamine and 2.73 g (0.021 mole) of 2-aminoethylmorpholine are successively added, and the reaction mixture is boiled for one hour. Upon cooling triethylamine hydrochloride gets separated, which is filtered and washed with 2-propanol. The filtrate is evaporated to dryness in vacuo and the residue is dissolved in chloroform. The solution thus obtained is extracted twice with water, dried over anhydrous Na2SO4 and evaporated in vacuo. The oily product is suspended in ethyl acetate, the crystalline product thus obtained is filtered off and washed with ethyl acetate.

Workup

  1. additionare successively added
  2. customgets separated
  3. filtrationwhich is filtered
  4. washwashed with 2-propanol
  5. customThe filtrate is evaporated to dryness in vacuo
  6. dissolutionthe residue is dissolved in chloroform
  7. customThe solution thus obtained
  8. extractionis extracted twice with water
  9. dry with materialdried over anhydrous Na2SO4
  10. customevaporated in vacuo
  11. customthe crystalline product thus obtained
  12. filtrationis filtered off
  13. washwashed with ethyl acetate

Sources & evidence

ORD record
ord-bad2392ba57a4117af7ac89f50d16c08
Source dataset
uspto-grants-1995_12
Patent number
US05478825

Reaction notes

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