Ammonium Chloride → HCID 20257267, compound

HRID 1105979Notes

Reaction equation

HRID 1105979 reaction equation
[CH3:1][O:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([N+:12]([O-])=O)=[CH:8][C:7]=1[S:15]([OH:18])(=[O:17])=[O:16].[Cl-].[NH4+]>O>[NH2:12][C:9]1[CH:10]=[CH:11][C:6]([O:5][CH2:4][CH2:3][O:2][CH3:1])=[C:7]([S:15]([OH:18])(=[O:17])=[O:16])[CH:8]=1

Participants

4

Reactant 2

HCID 25517Ammonium ChlorideHCID 12931436HCID 12931436, compound

Product 1

HCID 20257267HCID 20257267, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A mixture composed of 30 g of 2-(2-methoxyethoxy)-5-nitrobenzenesulfonic acid, 30 g of reduced iron, 0.6 g of ammonium chloride and 60 ml of water was kept at about 80° to 85° C. and stirred for 2 hours. After conclusion of the reaction, insoluble materials were removed by filtration, and 200 ml of isopropyl alcohol was added to the filtrate, which was cooled with ice. The crystals thus-formed were separated by filtration, washed with 50 ml of isopropyl alcohol and dried in the air. Yield: 23 g. m.p.: more than 250° C.

Workup

  1. customwas kept at about 80° to 85° C.
  2. customAfter conclusion of the reaction, insoluble materials
  3. customwere removed by filtration, and 200 ml of isopropyl alcohol
  4. additionwas added to the filtrate, which
  5. temperaturewas cooled with ice
  6. customThe crystals thus-formed
  7. customwere separated by filtration
  8. washwashed with 50 ml of isopropyl alcohol
  9. customdried in the air

Sources & evidence

ORD record
ord-e25757203b3243588f2104851328f4d2
Source dataset
uspto-grants-1982_01
Patent number
US04310693

Reaction notes

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