Hydrochloric Acid → HCID 19990248, compound

HRID 346074Notes

Reaction equation

HRID 346074 reaction equation
[CH2:1]([N:8]1[CH:12]=[C:11]([N+:13]([O-])=O)[C:10]([NH:16][CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:24]>[Pd]>[ClH:24].[ClH:24].[NH2:13][C:11]1[C:10]([NH:16][CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[N:9][N:8]([CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH:12]=1

Participants

4

Reactant 2

HCID 313Hydrochloric Acid2×HCID 19437615HCID 19437615, compound

Product 1

HCID 19990248HCID 19990248, compound

Reagents, catalysts & solvents 1

HCID 23938PalladiumCatalyst

Procedure

500 mg (1.62 mmoles) of 1-benzyl-3-benzylamino-4-nitropyrazol (Example 1, Step I, Fraction 1) are hydrated in 20 ml 5-normal methanolic hydrochloric acid with catalytic quantities of palladium/carbon at room temperature and 50 bar. After 17 hours, the hydration is concluded and hydrogen chloride gas is guided through the solution for 5 minutes. The solution is reduced in the rotary evaporator in a vacuum to half of the original volume and then mixed with acetic acid until a colorless precipitate is formed which is recrystallized from acetic acid/methanol.

Workup

  1. customThe solution is reduced in the rotary evaporator in a vacuum to half of the original volume
  2. additionmixed with acetic acid until a colorless precipitate
  3. customis formed which
  4. customis recrystallized from acetic acid/methanol

Sources & evidence

ORD record
ord-4646fe9dcb684923b64b0907d96a6bce
Source dataset
uspto-grants-1991_10
Patent number
US05061289

Reaction notes

Loading…