Ammonium Chloride → HCID 15511753, compound

HRID 1018907Notes

Reaction equation

HRID 1018907 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, rinsed with water and dried 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. washrinsed with water
  6. customdried

Sources & evidence

ORD record
ord-5d4c76cbf939460aa5ffa3709b388caa
Source dataset
uspto-grants-2002_11
Patent number
US06486143B2

Reaction notes

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