Hydrochloric Acid → 6-[2-(1-Pyrrolidinyl)ethylamino]-7,8,9,10-tetrahydro-1,2,4-triazolo[3,4-a]phthalazine hydrochloride hydrate

HRID 1154016Notes

Reaction equation

HRID 1154016 reaction equation
[N:1]1([CH2:6][CH2:7][NH:8][C:9]2[C:18]3[CH2:17][CH2:16][CH2:15][CH2:14][C:13]=3[C:12]3=[N:19][N:20]=[CH:21][N:11]3[N:10]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.[ClH:22].CC([OH:26])C>>[OH2:26].[ClH:22].[N:1]1([CH2:6][CH2:7][NH:8][C:9]2[C:18]3[CH2:17][CH2:16][CH2:15][CH2:14][C:13]=3[C:12]3=[N:19][N:20]=[CH:21][N:11]3[N:10]=2)[CH2:2][CH2:3][CH2:4][CH2:5]1

Participants

4

Reactant 3

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 133655886-[2-(1-Pyrrolidinyl)ethylamino]-7,8,9,10-tetrahydro-1,2,4-triazolo[3,4-a]phthalazine

Product 1

HCID 204360036-[2-(1-Pyrrolidinyl)ethylamino]-7,8,9,10-tetrahydro-1,2,4-triazolo[3,4-a]phthalazine hydrochloride hydrate

Procedure

A solution of 20.0 g of 6-[2-(1-pyrrolidinyl)ethylamino]-7,8,9,10-tetrahydro-1,2,4-triazolo[3,4-a]phthalazine in 60 ml of 2-propanol was heated to reflux and 6 ml of concentrated hydrochloric acid was added slowly. An exothermic reaction took place and a white precipitate formed immediately. The mixture was refluxed for 30 minutes and then cooled. The solid was separated by filtration, washed thoroughly with 2-propanol and then dried at 50° C. under reduced pressure to give 6-[2-(1-pyrrolidinyl)ethylamino]-7,8,9,10-tetrahydro-1,2,4-triazolo[3,4-a]phthalazine hydrochloride hydrate.

Workup

  1. temperatureto reflux
  2. customAn exothermic reaction
  3. customa white precipitate formed immediately
  4. temperatureThe mixture was refluxed for 30 minutes
  5. temperaturecooled
  6. customThe solid was separated by filtration
  7. washwashed thoroughly with 2-propanol
  8. customdried at 50° C. under reduced pressure

Sources & evidence

ORD record
ord-4801b8c01f5c4cdaa9a64976b3727b7d
Source dataset
uspto-grants-1984_12
Patent number
US04487930

Reaction notes

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