1-[2-(1,4-Benzodioxan-2-yl)-2-hydroxyethyl]-4-[(2,6-dimethylphenyl)aminocarbonylmethyl]piperazine acetate → HCID 13578745, compound

HRID 637778Notes

Reaction equation

HRID 637778 reaction equation
C(O)(=O)C.[O:5]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[O:8][CH2:7][CH:6]1[CH:15]([OH:35])[CH2:16][N:17]1[CH2:22][CH2:21][N:20]([CH2:23][C:24]([NH:26][C:27]2[C:32]([CH3:33])=[CH:31][CH:30]=[CH:29][C:28]=2[CH3:34])=[O:25])[CH2:19][CH2:18]1>S(=O)(=O)(O)O>[O:5]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[O:8][CH2:7][CH:6]1[CH:15]([OH:35])[CH2:16][N:17]1[CH2:18][CH2:19][N:20]([CH2:23][C:24]([NH:26][C:27]2[C:28]([CH3:34])=[CH:29][CH:30]=[CH:31][C:32]=2[CH3:33])=[O:25])[CH2:21][CH2:22]1

Participants

3

Reactant 1

HCID 704881351-[2-(1,4-Benzodioxan-2-yl)-2-hydroxyethyl]-4-[(2,6-dimethylphenyl)aminocarbonylmethyl]piperazine acetate

Product 1

HCID 13578745HCID 13578745, compound

Reagents, catalysts & solvents 1

HCID 1118Sulfuric AcidSolvent

Procedure

1-[2-(1,4-benzodioxan-2-yl)-2-hydroxyethyl]-4-[(2,6-dimethylphenyl)aminocarbonylmethyl]piperazine acetate (1.0 g) is dissolved in 50 ml 50% aqueous sulfuric acid, and the solution evaporated to dryness. The product is suspended in ethanol and filtered, air dried and recrystallized from methanol/acetone to yield 1-[2-(1,4-benzodioxan-2-yl)-2-hydroxyethyl]-4-[(2,6-dimethylphenyl)aminocarbonylmethyl]piperazine .2HSO4.

Workup

  1. customthe solution evaporated to dryness
  2. filtrationfiltered
  3. customair dried
  4. customrecrystallized from methanol/acetone

Sources & evidence

ORD record
ord-249fbf2411e64448a15ec7ed6fa4023e
Source dataset
uspto-grants-1985_12
Patent number
US04558129

Reaction notes

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