Ammonium Chloride → HCID 21322801, compound

HRID 26342

Reaction equation

HRID 26342 reaction equation
[Cl-].[NH4+].[Cl:3][C:4]1[CH:16]=[C:15]([N+:17]([O-])=O)[CH:14]=[CH:13][C:5]=1[NH:6][CH2:7][CH:8]1[O:12][CH2:11][CH2:10][CH2:9]1>[Zn]>[ClH:3].[Cl:3][C:4]1[CH:16]=[C:15]([NH2:17])[CH:14]=[CH:13][C:5]=1[NH:6][CH2:7][CH:8]1[O:12][CH2:11][CH2:10][CH2:9]1

Participants

4

Reactant 2

HCID 25517Ammonium ChlorideHCID 213228042-chloro-4-nitro-N-tetrahydrofurfurylaniline

Product 1

HCID 21322801HCID 21322801, compound

Reagents, catalysts & solvents 1

HCID 23994ZincCatalyst

Procedure

3.0 g of ammonium chloride and 50 g of zinc powder are added to 150 ml of an aqueous-alcoholic solution (85% of alcohol and 15% of water). This mixture is heated to the reflux temperature, whilst stirring, and 0.1 mol (25.7 g) of 2-chloro-4-nitro-N-tetrahydrofurfurylaniline is then added gradually. When the addition has ended and the reaction mixture is decolorised, the latter is filtered and the filtrate is collected in 20 ml of ice-cooled hydrochloric acid. After cooling, the expected hydrochloride precipitates in the form of crystals. It is filtered off, washed with a small amount of ice-cooled absolute alcohol and dried in vacuo. It melts at about 170° C. with decomposition.

Workup

  1. temperatureThis mixture is heated to the reflux temperature
  2. additionWhen the addition
  3. filtrationthe latter is filtered
  4. customthe filtrate is collected in 20 ml of ice-
  5. temperaturecooled hydrochloric acid
  6. temperatureAfter cooling
  7. customthe expected hydrochloride precipitates in the form of crystals
  8. filtrationIt is filtered off
  9. washwashed with a small amount of ice-
  10. temperaturecooled absolute alcohol
  11. customdried in vacuo

Sources & evidence

ORD record
ord-7b37cd148ced4afebf90ae56e028634c
Source dataset
uspto-grants-1979_04
Patent number
US04149848

Linked notes

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