Methylamine → HCID 13376801, compound

HRID 1980087Notes

Reaction equation

HRID 1980087 reaction equation
Cl[C:2]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[C:5]2=[N:12][N:13]=[N:14][N:4]2[N:3]=1.[CH3:15][NH2:16]>CO>[CH3:15][NH:16][C:2]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[C:5]2=[N:12][N:13]=[N:14][N:4]2[N:3]=1

Participants

4

Reactant 2

HCID 6329MethylamineHCID 133767996-Chloro-7,8,9,10-tetrahydrotetrazolo[5,1-a]phthalazine

Product 1

HCID 13376801HCID 13376801, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A mixture of 6.0 g of 6-chloro-7,8,9,10-tetrahydrotetrazolo[5,1-a]phthalazine and 125 ml of 40% aqueous methylamine in 15 ml of methanol was heated under reflux for 3 hours. The reaction mixture was then cooled and the crystalline solid present was separated by filtration. It was recrystallized from a mixture of dimethylsulfoxide and water to give 6-methylamino-7,8,9,10-tetrahydrotetrazolo[5,1-a]phthalazine melting at about 318° C.

Workup

  1. temperaturewas heated
  2. temperatureunder reflux for 3 hours
  3. temperatureThe reaction mixture was then cooled
  4. customthe crystalline solid present was separated by filtration
  5. customIt was recrystallized from a mixture of dimethylsulfoxide and water

Sources & evidence

ORD record
ord-d6e46d352d6947f8833e014629b24089
Source dataset
uspto-grants-1984_11
Patent number
US04485106

Reaction notes

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