Ammonia → HCID 13359830, compound

HRID 616758Notes

Reaction equation

HRID 616758 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:9]2[C:21]([CH3:22])=[N:20][N:19]([CH3:23])[C:10]=2[N:11]=[C:12]([NH:15][CH2:16][C:17]#[CH:18])[CH2:13][N:14]=1.S(=O)(=O)(O)O.N>>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:9]2[C:21]([CH3:22])=[N:20][N:19]([CH3:23])[C:10]=2[N:11]2[C:17]([CH3:18])=[CH:16][N:15]=[C:12]2[CH2:13][N:14]=1

Participants

4

Reactant 3

HCID 222AmmoniaHCID 1118Sulfuric AcidHCID 178456822HCID 178456822, compound

Product 1

HCID 13359830HCID 13359830, compound

Procedure

With stirring, 1.4 g. of 4-(2-chlorophenyl)-1,6-dihydro-1,3-dimethyl-7-(2-propynylamino)pyrazolo[3,4-e][1,4]-diazepine is dissolved in a solution of 1 mg. of mercuric oxide in 5 ml. of concentrated sulfuric acid at 50° C. The solution is allowed to stand for 16 hours at room temperature (20°-30° C.), then is poured over crushed ice and basified with excess concentrated aqueous ammonia. The mixture is extracted repeatedly with dichloromethane. The extracts are combined, dried and evaporated at reduced pressure to give a residue of 4-(2-chlorophenyl)-1,6-dihydro-1,3,9-trimethylimidazo-[1,2-a]pyrazolo[4,3-f][1,4]diazepine; m.p. 189-190° C. (dec.) after sublimation at 130° C. and 0.1 mm. Hg.

Workup

  1. customat 50° C
  2. addition(20°-30° C.), then is poured
  3. customover crushed ice
  4. extractionThe mixture is extracted repeatedly with dichloromethane
  5. customdried
  6. customevaporated at reduced pressure

Sources & evidence

ORD record
ord-d852e6adbd4243cea6edf64d88d313b8
Source dataset
uspto-grants-1978_02
Patent number
US04075408

Reaction notes

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