Azane;hydrate → HCID 20339008, compound

HRID 1395344Notes

Reaction equation

HRID 1395344 reaction equation
C[O:2][C:3](=O)[CH:4]([O:6][C:7]1[CH:12]=[C:11]([O:13][C:14]2[CH:19]=[CH:18][C:17]([C:20]([F:23])([F:22])[F:21])=[CH:16][C:15]=2[Cl:24])[CH:10]=[CH:9][C:8]=1[C:25]#[N:26])[CH3:5].O.[NH3:29]>C1C=CC=CC=1>[C:25]([C:8]1[CH:9]=[CH:10][C:11]([O:13][C:14]2[CH:19]=[CH:18][C:17]([C:20]([F:22])([F:23])[F:21])=[CH:16][C:15]=2[Cl:24])=[CH:12][C:7]=1[O:6][CH:4]([CH3:5])[C:3]([NH2:29])=[O:2])#[N:26]

Participants

4

Reactant 2

HCID 12896473Azane;hydrateHCID 13255940HCID 13255940, compound

Product 1

HCID 20339008HCID 20339008, compoundYield 57.1%

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Conditions

Temperature
0 °C

Procedure

A 10 g of methyl-α-[2-cyano-5-(2-chloro-4-trifluoromethyl phenoxy)phenoxy]propionate was dissolved in 20 ml of benzene. The solution was cooled at 0° C. and 10 g of 28% ammonia water was added dropwise to react them at room temperature for 2 hours. After the reaction, the benzene phase was separated and was washed with water. The benzene was distilled off and the product was recrystallized from methanol to obtain 5.5 g of the object compound having a melting point of 134° to 137° C.

Workup

  1. customto react them at room temperature for 2 hours
  2. customAfter the reaction
  3. customthe benzene phase was separated
  4. washwas washed with water
  5. distillationThe benzene was distilled off
  6. customthe product was recrystallized from methanol

Sources & evidence

ORD record
ord-4189976cfb434aceada7a1f2444bc860
Source dataset
uspto-grants-1980_05
Patent number
US04203758

Reaction notes

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