Hydrazine → HCID 131714395, compound

HRID 465099Notes

Reaction equation

HRID 465099 reaction equation
[IH:1].[CH3:2][C:3]1([CH3:14])[CH2:9][CH2:8][C:7]([CH3:11])([CH3:10])[NH:6][C:5](SC)=[N:4]1.[NH2:15][NH2:16]>C(O)C.CCOCC>[IH:1].[NH:15]([C:5]1[NH:6][C:7]([CH3:11])([CH3:10])[CH2:8][CH2:9][C:3]([CH3:14])([CH3:2])[N:4]=1)[NH2:16]

Participants

5

Reactant 2

HCID 9321HydrazineHCID 2797333HCID 2797333, compound

Product 1

HCID 131714395HCID 131714395, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 3283Diethyl EtherSolvent

Procedure

A 10.0 g portion of 4,5,6,7-tetrahydro-4,4,7,7-tetramethyl-2-methylthio-1H-1,3-diazepine, hydroiodide was dissolved in 150 ml of ethanol and 2.5 g of hydrazine was added. The mixture was refluxed 6 hours, diluted with 300 ml of ether and stored at -10° C. The solid was removed by filtration. The filtrate was concentrated to about 25 ml in vacuo, diluted with 50 ml of 2-propanol, then 200 ml of ether and stored at -10° C. The solid was collected, washed with ether and dried in vacuo at 60° C., giving 3.5 g of the desired intermediate, mp 154°-155° C.

Workup

  1. temperatureThe mixture was refluxed 6 hours
  2. customstored at -10° C
  3. customThe solid was removed by filtration
  4. concentrationThe filtrate was concentrated to about 25 ml in vacuo
  5. additiondiluted with 50 ml of 2-propanol
  6. customstored at -10° C
  7. customThe solid was collected
  8. washwashed with ether
  9. customdried in vacuo at 60° C.

Sources & evidence

ORD record
ord-bbabb21d143948cd80c99d710f6758e5
Source dataset
uspto-grants-1985_10
Patent number
US04550169

Reaction notes

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