Tert-Butylamine → HCID 12671207, compound

HRID 435982Notes

Reaction equation

HRID 435982 reaction equation
[Cl:1][C:2]1[N:7]2[N:8]=[CH:9][N:10]=[C:6]2[N:5]=[C:4]([CH3:11])[C:3]=1[CH2:12][CH:13](Cl)[CH3:14].[C:16]([NH2:20])([CH3:19])([CH3:18])[CH3:17].C(=O)([O-])[O-].[Na+].[Na+].Cl.C(O)C>C(O)C>[ClH:1].[C:16]([N:20]1[C:2]2[N:7]3[N:8]=[CH:9][N:10]=[C:6]3[N:5]=[C:4]([CH3:11])[C:3]=2[CH2:12][CH:13]1[CH3:14])([CH3:19])([CH3:18])[CH3:17]

Participants

6

Reactant 4

HCID 6385Tert-ButylamineHCID 10340Sodium CarbonateHCID 126712987-Chloro-6-(2-chloropropyl)-5-methyl[1,2,4]triazolo[1,5-a]pyrimidineHCID 21887872Ethanol hydrochloride

Product 1

HCID 12671207HCID 12671207, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A mixture of 2.4g of 7-chloro-6-(2-chloropropyl)-5-methyl-s-triazolo[1,5-a]pyrimidine, 0.9g of tert-butylamine, 1.8g of sodium carbonate and 20 ml of ethanol was stirred for 3 hours at room temperature and then refluxed for 5 hours. The hot reaction mixture was filtered, the filtrate was concentrated under reduced pressure and the residue was purified by a column chromatography of alumina. To an oily substance thus obtained was added a solution of hydrogen chloride-ethanol and the crystals precipitated thereby were collected by filtration.

Workup

  1. temperaturerefluxed for 5 hours
  2. filtrationThe hot reaction mixture was filtered
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customthe residue was purified by a column chromatography of alumina
  5. customTo an oily substance thus obtained
  6. customthe crystals precipitated
  7. filtrationthereby were collected by filtration

Sources & evidence

ORD record
ord-1cfee84882404cb2b9c29876088a09f9
Source dataset
uspto-grants-1977_02
Patent number
US04007189

Reaction notes

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