Chloral Hydrate → HCID 73668067, compound

HRID 1755680Notes

Reaction equation

HRID 1755680 reaction equation
[Cl:1][C:2]([Cl:7])([Cl:6])[CH:3](O)[OH:4].[Cl:8][C:9]1[N:14]=[CH:13][C:12]([CH2:15][N:16]([C:18]([NH:23][CH3:24])=[CH:19][N+:20]([O-:22])=[O:21])[CH3:17])=[CH:11][CH:10]=1.C(N(CC)CC)C>C(#N)C>[Cl:1][C:2]([Cl:7])([Cl:6])[CH:3]([OH:4])[C:19]([N+:20]([O-:22])=[O:21])=[C:18]([N:16]([CH2:15][C:12]1[CH:13]=[N:14][C:9]([Cl:8])=[CH:10][CH:11]=1)[CH3:17])[NH:23][CH3:24]

Participants

5

Reactant 3

HCID 2707Chloral HydrateHCID 8471TriethylamineHCID 85054604N-[(6-Chloro-3-pyridinyl)methyl]-N,N′-dimethyl-2-nitro-1,1-ethenediamine

Product 1

HCID 73668067HCID 73668067, compound

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

Chloral hydrate (0.40 g) was added slowly in 40 minutes to a mixture of 1-[N-(6-chloro-3-pyridylmethyl)-N-methylamino]-1-methylamino-2-nitroethylene (0.26 g), triethylamine (0.1 g) and acetonitrile (3 ml). The mixture was stirred at room temperature for 21 hours and under refluxing for 9 hours. The resultant crystals were collected by filtration to give 1,1,1-trichloro-4-[N-(6-chloro-3-pyridylmethyl)-N-methylamino]-4-methylamino-3-nitro-3-buten-2-ol (Compound No. 11) (0.23 g) as a white solid.

Workup

  1. temperatureunder refluxing for 9 hours
  2. filtrationThe resultant crystals were collected by filtration

Sources & evidence

ORD record
ord-1ff890c3c78b4785bb77c8a88bfd7899
Source dataset
uspto-grants-1995_08
Patent number
US05438065

Reaction notes

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