Methane → HCID 15541455, compound

HRID 1597292Notes

Reaction equation

HRID 1597292 reaction equation
[CH:1]1([C:4]2[NH:12][C:11]3[C:10](=S)[NH:9][C:8](=[S:14])[N:7]([CH2:15][CH3:16])[C:6]=3[N:5]=2)[CH2:3][CH2:2]1.[CH2:17]([NH2:19])[CH3:18].C>O>[CH:1]1([C:4]2[NH:12][C:11]3[C:10]([NH:19][CH2:17][CH3:18])=[N:9][C:8](=[S:14])[N:7]([CH2:15][CH3:16])[C:6]=3[N:5]=2)[CH2:3][CH2:2]1

Participants

5

Conditions

Temperature
150 °C

Procedure

8-cyclopropyl-3-ethyl-2,6-dithioxanthine (20.19 g) prepared according to the method of example 2(i), and 70% ethylamine in water (320 ml 4.0M) were placed in a 450 ml pressure reactor and heated to 150° C. for 6 hours. The reaction solution was cooled to room temperature, treated with 2 portions of charcoal (0.2 g) filtered, and evaporated to dryness. The residue was triturated in methanol (300 ml), concentrated to about 200 ml and the solid collected (16.48 g), mp 265 with decomposition.

Workup

  1. customwere placed in a 450 ml pressure reactor
  2. temperatureThe reaction solution was cooled to room temperature
  3. filtrationfiltered
  4. customevaporated to dryness
  5. customThe residue was triturated in methanol (300 ml)
  6. concentrationconcentrated to about 200 ml
  7. customthe solid collected (16.48 g), mp 265 with decomposition

Sources & evidence

ORD record
ord-361064c9915a44dfa94d91827ffeb373
Source dataset
uspto-grants-2001_09
Patent number
US06294541B1

Reaction notes

Loading…