Nicotinic Acid → HCID 86733169, compound

HRID 267910Notes

Reaction equation

HRID 267910 reaction equation
[CH3:1][CH2:2][CH2:3][CH2:4][CH:5]([CH2:8][N:9]1[CH2:14][N:13]([CH2:15][CH:16]([CH2:19][CH2:20][CH2:21][CH3:22])[CH2:17][CH3:18])[CH2:12][C:11]([NH2:24])([CH3:23])[CH2:10]1)[CH2:6][CH3:7].[C:25]([OH:33])(=[O:32])[C:26]1[CH:31]=[CH:30][CH:29]=[N:28][CH:27]=1>CO>[CH3:22][CH2:21][CH2:20][CH2:19][CH:16]([CH2:15][N:13]1[CH2:14][N:9]([CH2:8][CH:5]([CH2:4][CH2:3][CH2:2][CH3:1])[CH2:6][CH3:7])[CH2:10][C:11]([NH2:24])([CH3:23])[CH2:12]1)[CH2:17][CH3:18].[C:25]([O-:33])(=[O:32])[C:26]1[CH:31]=[CH:30][CH:29]=[N:28][CH:27]=1

Participants

4

Reactant 2

HCID 938Nicotinic AcidHCID 3607Hexetidine

Product 1

HCID 86733169HCID 86733169, compoundYield 70%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Conditions

Temperature
50 °C

Procedure

Hexetidine (1 mole) was dissolved in 1,000 ml methanol and heated to 50°C. To the solution nicotinic acid (1 mole) was added dropwise. After stirring for 1.5 hours at 50°C, half of the solvent was distilled off under vacuum at 40°C. The crystal slurry obtained at room temperature was filtered and recrystallized from acetic acid ethyl ester, yielding hexetidine nicotinate as white crystals.

Workup

  1. distillationhalf of the solvent was distilled off under vacuum at 40°C
  2. customThe crystal slurry obtained at room temperature
  3. filtrationwas filtered
  4. customrecrystallized from acetic acid ethyl ester

Sources & evidence

ORD record
ord-f31a20a8b645417d9ff9c37ac91f2b33
Source dataset
uspto-grants-1976_03
Patent number
US03946013

Reaction notes

Loading…