Hydrochloric Acid → HCID 70573459, compound

HRID 1390066Notes

Reaction equation

HRID 1390066 reaction equation
[CH2:1]([NH:5][C:6]1[CH:7]=[C:8]([CH:12]=[C:13]([S:22](=[O:25])(=[O:24])[NH2:23])[C:14]=1[O:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[CH:9]=[N:10]O)[CH2:2][CH2:3][CH3:4].[ClH:26]>C(O)(=O)C>[ClH:26].[CH2:1]([NH:5][C:6]1[CH:7]=[C:8]([CH:12]=[C:13]([S:22](=[O:25])(=[O:24])[NH2:23])[C:14]=1[O:15][C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1)[CH2:9][NH2:10])[CH2:2][CH2:3][CH3:4]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 86735607HCID 86735607, compound

Product 1

HCID 70573459HCID 70573459, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

A mixture of 3-n-butylamino-4-phenoxy-5-sulfamylbenzaldoxime (3.6 g), stannous chloride dihydrate (12 g), concentrated hydrochloric acid (25 ml) and acetic acid (50 ml) is heated on a steam-bath for 2-3 hours. After concentration in vacuo to about 50 ml, 3-n-butylamino-4-phenoxy-5-sulfamylbenzylamine hydrochloride starts to crystallize from the solution. After cooling, the hydrochloride is collected by filtration, washed with ethanol and dried in air. After recrystallization from 2-methoxyethanol it is obtained with a melting point higher than 300° C.

Workup

  1. temperatureis heated on a steam-bath for 2-3 hours
  2. concentrationAfter concentration in vacuo to about 50 ml, 3-n-butylamino-4-phenoxy-5-sulfamylbenzylamine hydrochloride
  3. customto crystallize from the solution
  4. temperatureAfter cooling
  5. filtrationthe hydrochloride is collected by filtration
  6. washwashed with ethanol
  7. customdried in air
  8. customAfter recrystallization from 2-methoxyethanol it
  9. customis obtained with a melting point higher than 300° C.

Sources & evidence

ORD record
ord-29f521e3fe2c486ca0e7b41674a21dd0
Source dataset
uspto-grants-1981_01
Patent number
US04247550

Reaction notes

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