Hydrazine hydrate (1:1) → HCID 70269738, compound

HRID 1274825Notes

Reaction equation

HRID 1274825 reaction equation
C[O:2][C:3](=O)[C:4]1[CH:9]=[C:8]([O:10][CH3:11])[CH:7]=[C:6]([O:12][C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([O:19][C:20]([F:23])([F:22])[F:21])[CH:14]=2)[N:5]=1.O.[NH2:26][NH2:27]>CO>[CH3:11][O:10][C:8]1[CH:7]=[C:6]([O:12][C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([O:19][C:20]([F:23])([F:22])[F:21])[CH:14]=2)[N:5]=[C:4]([C:3]([NH:26][NH2:27])=[O:2])[CH:9]=1

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 53777509HCID 53777509, compound

Product 1

HCID 70269738HCID 70269738, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

4-methoxy-6-[3-(trifluoromethoxy)phenoxy] picolinic acid methyl ester (0.74 g, 0.00216 mol) was dissolved in methanol (about 10 ml), and then mixed with hydrazine monohydrate (1.08 g, 0.00216×10 mol). The resultant mixture was refluxed for about 3 hours. The obtained reaction solution was concentrated and dissolved in ethyl acetate, and then distributed in ethyl acetate-saturated sodium bicarbonate water. The organic phase separated from the solution was washed with saturated brine, dried with anhydrous sodium sulfate and then concentrated, thereby obtaining an aimed product.

Workup

  1. customThe obtained reaction solution
  2. concentrationwas concentrated
  3. dissolutiondissolved in ethyl acetate
  4. customThe organic phase separated from the solution
  5. washwas washed with saturated brine
  6. dry with materialdried with anhydrous sodium sulfate
  7. concentrationconcentrated

Sources & evidence

ORD record
ord-465873742a544b1ea18925dcbdcae51d
Source dataset
uspto-grants-2000_12
Patent number
US06159901

Reaction notes

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