Ammonium Chloride → HCID 15511753, compound

HRID 1358204Notes

Reaction equation

HRID 1358204 reaction equation
[CH2:1]([O:3][P:4]([C:9]1[C:10](=[O:23])[NH:11][C:12]2[C:17]([CH:18]=1)=[CH:16][C:15]([N+:19]([O-])=O)=[C:14]([Cl:22])[CH:13]=2)(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2].[Cl-].[NH4+]>CO.O.[Fe]>[CH2:1]([O:3][P:4]([C:9]1[C:10](=[O:23])[NH:11][C:12]2[C:17]([CH:18]=1)=[CH:16][C:15]([NH2:19])=[C:14]([Cl:22])[CH:13]=2)(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2]

Participants

6

Reactant 2

HCID 25517Ammonium ChlorideHCID 15511752HCID 15511752, compound

Product 1

HCID 15511753HCID 15511753, compound

Reagents, catalysts & solvents 3

HCID 23925IronCatalystHCID 887MethanolSolventHCID 962WaterSolvent

Procedure

A suspension of the compound obtained in Step C (7.0 g, 19.4 mmol), powdered iron (10.8 g, 194 mmol) and ammonium chloride (10.4 g, 194 mmol) is stirred at reflux for 1 hour in a mixture of 270 ml of methanol and 90 ml of water. The suspension is filtered hot over Celite and the solid is rinsed several times with methanol. The filtrate is evaporated to dryness and the residue is suspended in water. The solid is filtered off, rinsing with water and drying to obtain the title product in the form of orange crystals.

Workup

  1. filtrationThe suspension is filtered hot over Celite
  2. washthe solid is rinsed several times with methanol
  3. customThe filtrate is evaporated to dryness
  4. filtrationThe solid is filtered off
  5. washrinsing with water
  6. customdrying

Sources & evidence

ORD record
ord-da60363f96fc46ea9bdb37ed70a07efb
Source dataset
uspto-grants-2003_07
Patent number
US06596709B1

Reaction notes

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