Water → HCID 25193405, compound

HRID 2366459Notes

Reaction equation

HRID 2366459 reaction equation
[NH2:1][C:2]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][C:7]([F:13])=[CH:6][C:3]=1[C:4]#[N:5].[OH2:14]>ClCCl>[NH2:1][C:2]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][C:7]([F:13])=[CH:6][C:3]=1[C:4]([NH2:5])=[O:14]

Participants

4

Reactant 2

HCID 962WaterHCID 25194664HCID 25194664, compound

Product 1

HCID 25193405HCID 25193405, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A suspension of EXAMPLE 45B (13.9 g) in polyphosphoric acid (400 g) was stirred at 115° C. for 3 hours. After cooling, water and dichloromethane were added and the mixture stirred at ambient temperature for 10 minutes. The solid material was collected by filtration and recrystallized from methanol.

Workup

  1. temperatureAfter cooling
  2. filtrationThe solid material was collected by filtration
  3. customrecrystallized from methanol

Sources & evidence

ORD record
ord-396383b33c9840019b4f0ab85cb71e72
Source dataset
uspto-grants-2014_04
Patent number
US08697736B2

Reaction notes

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