HCID 15671294, compound → HCID 136110837, compound

HRID 2248108Notes

Reaction equation

HRID 2248108 reaction equation
CC1(C)[O:20][C:5]2=[CH:6][C:7]3[N:8]=[C:9]([C:17]([OH:19])=[O:18])[C:10]([C:14]([OH:16])=[O:15])=[N:11][C:12]=3[CH:13]=[C:4]2[O:3]1>Cl>[OH:3][C:4]1[CH:13]=[C:12]2[C:7](=[CH:6][C:5]=1[OH:20])[N:8]=[C:9]([C:17]([OH:19])=[O:18])[C:10]([C:14]([OH:16])=[O:15])=[N:11]2

Participants

3

Conditions

Temperature
75 °C

Procedure

Compound from Example 3E (145 mg, 0.5 mmole) was slurried in 10 ml of concentrated HCl and heated at 75° C. for 1 hour with stirring. On initial heating, the compound dissolved, then a precipitate eventually formed. The slurry was evaporated to dryness in vacuo. The residue was initially soluble in water but formed a yellow-brown precipitate within a few minutes. The water was evaporated again and the residue was dried in vacuo for 3 hours to give the title compound as a brown solid, 125 mg, m.p. >300° C.

Workup

  1. temperatureOn initial heating
  2. dissolutionthe compound dissolved
  3. customa precipitate eventually formed
  4. customThe slurry was evaporated to dryness in vacuo
  5. customformed a yellow-brown precipitate within a few minutes
  6. customThe water was evaporated again
  7. customthe residue was dried in vacuo for 3 hours

Sources & evidence

ORD record
ord-28684ef8beca45b5ada38db93633cad2
Source dataset
uspto-grants-1991_08
Patent number
US05037983

Reaction notes

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