Methylhydrazine → HCID 11743328, compound

HRID 976341Notes

Reaction equation

HRID 976341 reaction equation
[CH3:1][C:2]1([CH3:31])[CH2:15][CH2:14][C:13]([CH3:17])([CH3:16])[C:12]2[CH:11]=[C:10]3[C:5]([CH2:6][CH2:7][CH:8]([C:19]([C:21]4[CH:30]=[CH:29][C:24]([C:25]([O:27][CH3:28])=[O:26])=[CH:23][CH:22]=4)=O)[C:9]3=O)=[CH:4][C:3]1=2.[CH3:32][NH:33][NH2:34]>CO>[CH3:32][N:33]1[C:9]2[C:10]3[C:5]([CH2:6][CH2:7][C:8]=2[C:19]([C:21]2[CH:30]=[CH:29][C:24]([C:25]([O:27][CH3:28])=[O:26])=[CH:23][CH:22]=2)=[N:34]1)=[CH:4][C:3]1[C:2]([CH3:1])([CH3:31])[CH2:15][CH2:14][C:13]([CH3:17])([CH3:16])[C:12]=1[CH:11]=3

Participants

4

Reactant 2

HCID 6061MethylhydrazineHCID 10251458HCID 10251458, compound

Product 1

HCID 11743328HCID 11743328, compoundYield 65.1%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

4.5 g of methyl 4-(3,4,5,6,7,8-hexahydro-5,5,8,8-tetramethyl-1(2H)-anthracenon-2-ylcarbonyl)benzoate was suspended in 100 ml of methanol, followed by the addition thereto of 0.64 g of monomethylhydrazine. The obtained mixture was heated under reflux for 2 hours and cooled by allowing to stand to precipitate a solid. This solid was recovered by filtration and washed with methanol. 3.0 g of the title compound was obtained as a pale-yellow solid.

Workup

  1. additionfollowed by the addition
  2. temperatureThe obtained mixture was heated
  3. temperatureunder reflux for 2 hours
  4. temperaturecooled
  5. customto precipitate a solid
  6. filtrationThis solid was recovered by filtration
  7. washwashed with methanol

Sources & evidence

ORD record
ord-00617ab212a84062a341277d44af6d9d
Source dataset
uspto-grants-1997_03
Patent number
US05612356

Reaction notes

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