Ammonia → HCID 21430459, compound

HRID 437163Notes

Reaction equation

HRID 437163 reaction equation
Cl.[CH3:2][N:3]([CH3:23])[S:4]([C:7]1[CH:8]=[C:9]([CH:13]=[CH:14][C:15]=1[N:16]1[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]1)[C:10](Cl)=[O:11])(=[O:6])=[O:5].[CH2:24]([OH:28])[CH2:25][CH2:26][CH3:27].N>O>[CH2:24]([O:28][C:10](=[O:11])[C:9]1[CH:13]=[CH:14][C:15]([N:16]2[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]2)=[C:7]([S:4](=[O:5])(=[O:6])[N:3]([CH3:23])[CH3:2])[CH:8]=1)[CH2:25][CH2:26][CH3:27]

Participants

5

Reactant 3

HCID 222AmmoniaHCID 2631-Butanol2×HCID 21430472HCID 21430472, compound

Product 1

HCID 21430459HCID 21430459, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

40 Grams of 3-dimethylsulfamoyl-4-(4-methylpiperazine-1-yl)-benzoylchloride-hydrochloride (0.1 mole) were heated under reflux for 2 hours with 0.4 l of n-butanol. Subsequently the n-butanol was eliminated in vacuo, the residue was dissolved in 0.5 l of water, and the pH value of the filtered solution was adjusted to 8.5 by means of 2N ammonia. The crystalline precipitate was suction-filtered, washed with water, then dried in vacuo at 40° C. and finally dissolved and reprecipitated from a mixture of acetic ester and diisopropylether.

Workup

  1. filtrationThe crystalline precipitate was suction-filtered
  2. washwashed with water
  3. customdried in vacuo at 40° C.
  4. dissolutionfinally dissolved
  5. customreprecipitated from a mixture of acetic ester and diisopropylether

Sources & evidence

ORD record
ord-5205ac4c40414da0ad4da36e1528e444
Source dataset
uspto-grants-1977_06
Patent number
US04029787

Reaction notes

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