Acetic Acid → HCID 19746916, compound

HRID 484267Notes

Reaction equation

HRID 484267 reaction equation
[CH3:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][C:3]=1[NH:11][C:12](=O)OCCCl.[OH-].[K+].[C:20](O)(=[O:22])C>O>[OH:22][CH2:20][CH2:12][NH:11][C:3]1[CH:4]=[CH:5][CH:6]=[C:7]([N+:8]([O-:10])=[O:9])[C:2]=1[CH3:1]

Participants

5

Reactant 3

HCID 176Acetic AcidHCID 14797Potassium HydroxideHCID 19746918HCID 19746918, compound

Product 1

HCID 19746916HCID 19746916, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
80 °C

Procedure

25.8 g of the β-chloroethyl N-(2-methyl-3-nitrophenyl)-carbamate prepared under Example 3, stage 1, are initially introduced into the reaction vessel in 250 ml of water. The reaction mixture is heated to 80° C. and 35 g of 50% strength aqueous potassium hydroxide solution are then added in the course of one hour. After the mixture has been subsequently stirred at 75° C. for 3 hours, its pH is brought to 8 with glacial acetic acid, and the reaction mixture is cooled slowly. The product which has precipitated is filtered off with suction, washed with water, and dried at 50° C. in a vacuum drying cabinet.

Workup

  1. temperaturethe reaction mixture is cooled slowly
  2. customThe product which has precipitated
  3. filtrationis filtered off with suction
  4. washwashed with water
  5. customdried at 50° C. in a vacuum
  6. customdrying cabinet

Sources & evidence

ORD record
ord-fa4dadc7610744dba6366a1e6d822c43
Source dataset
uspto-grants-1993_07
Patent number
US05230710

Reaction notes

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