Hydrochloric Acid → HCID 53693672, compound

HRID 1283473Notes

Reaction equation

HRID 1283473 reaction equation
[CH2:1]([O:6][C:7]1[N:12]=[C:11]([N:13]2[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)[N:10]=[C:9]([N:19]2[CH2:24][CH2:23][S:22][CH2:21][CH2:20]2)[C:8]=1[N+:25]([O-:27])=[O:26])[C:2]([CH3:5])([CH3:4])[CH3:3].Cl.[OH:29]O.[OH-].[Na+]>O>[CH2:1]([O:6][C:7]1[N:12]=[C:11]([N:13]2[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)[N:10]=[C:9]([N:19]2[CH2:20][CH2:21][S:22](=[O:29])[CH2:23][CH2:24]2)[C:8]=1[N+:25]([O-:27])=[O:26])[C:2]([CH3:5])([CH3:4])[CH3:3]

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 21517895HCID 21517895, compound

Product 1

HCID 53693672HCID 53693672, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

4.5 gm (0.011 mol) of 6-neopentyloxy-5-nitro-2-piperazino-4-thiomorpholino-pyrimidine were suspended in a mixture of 60 ml of water and 11.4 ml (0.022 mol) of 2 N hydrochloric acid. 1.66 gm (0.011 mol) of 30% hydrogen peroxide were added to the suspension, and the mixture was stirred for 24 hours at room temperature, whereby a clear solution was obtained. The solution was made alkaline by careful addition of 12 ml of 2 N sodium hydroxide, and the yellow precipitate formed thereby was suction-filtered off, washed with water and recrystallized from a mixture of 30 ml of methanol and 20 ml of water. Yield: 2.4 gm (51.2% of theory); m.p. 156°-158°C.

Workup

  1. customwhereby a clear solution was obtained
  2. customthe yellow precipitate formed
  3. filtrationthereby was suction-filtered off
  4. washwashed with water
  5. customrecrystallized from a mixture of 30 ml of methanol and 20 ml of water

Sources & evidence

ORD record
ord-05e37619b11f4766aa596a84640c4546
Source dataset
uspto-grants-1976_08
Patent number
US03975384

Reaction notes

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