Chloral Hydrate → HCID 6790533, compound

HRID 1762737Notes

Reaction equation

HRID 1762737 reaction equation
Cl[C:2](Cl)(Cl)[CH:3]([OH:5])O.S([O-])([O-])(=O)=O.[Na+].[Na+].[F:15][C:16]1[CH:17]=[C:18]([CH:20]=[CH:21][C:22]=1[F:23])[NH2:19].Cl.[NH2:25][OH:26]>O.Cl>[F:15][C:16]1[CH:17]=[C:18]([NH:19][C:3](=[O:5])[CH:2]=[N:25][OH:26])[CH:20]=[CH:21][C:22]=1[F:23]

Participants

7

Reactant 4

HCID 2707Chloral HydrateHCID 24436Sodium SulfateHCID 774693,4-DifluoroanilineHCID 443297Hydroxyamine hydrochloride

Product 1

HCID 6790533HCID 6790533, compoundYield 42%

Reagents, catalysts & solvents 2

HCID 313Hydrochloric AcidSolventHCID 962WaterSolvent2×

Procedure

A solution of 18.2 g of chloral hydrate and 260 g of anhydrous sodium sulfate in 400 ml of water was mixed with a solution of 12.9 g of 3,4-difluoroaniline and 22.24 g of hydroxylamine hydrochloride in 160 ml of water and 9 ml of concentrated hydrochloric acid. This reaction mixture was refluxed for 2 hours and then filtered while hot, collecting the solid which was washed well with water and dried. Recrystallization from hot water gave 8.4 g of the desired compound as colorless crystals, mp 148°-150° C.

Workup

  1. temperatureThis reaction mixture was refluxed for 2 hours
  2. filtrationfiltered while hot,
  3. customcollecting the solid which
  4. washwas washed well with water
  5. customdried
  6. customRecrystallization from hot water

Sources & evidence

ORD record
ord-a20620d2aa1b449ea15ef122f382d440
Source dataset
uspto-grants-1989_05
Patent number
US04833270

Reaction notes

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