Methanesulfonic Acid → HCID 131711652, compound

HRID 46476Notes

Reaction equation

HRID 46476 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12]([CH2:13][CH2:14][CH2:15][N:16]([CH3:18])[CH3:17])[N:11]=[C:10]3[C:19]4[C:24]([CH2:25][C:9]=23)=[CH:23][CH:22]=[CH:21][CH:20]=4)=[CH:4][CH:3]=1.[CH3:26][S:27]([OH:30])(=[O:29])=[O:28]>CC#N>[CH3:26][S:27]([OH:30])(=[O:29])=[O:28].[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:12]([CH2:13][CH2:14][CH2:15][N:16]([CH3:18])[CH3:17])[N:11]=[C:10]3[C:19]4[C:24]([CH2:25][C:9]=23)=[CH:23][CH:22]=[CH:21][CH:20]=4)=[CH:6][CH:7]=1

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 203872963-(4-chlorophenyl)-N,N-dimethylindeno[1,2-c]pyrazole-2(4H)-propanamine

Product 1

HCID 131711652HCID 131711652, compound

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent2×

Procedure

A solution of 4.9 g (0.0139 mole) of the free base, 3-(4-chlorophenyl)-N,N-dimethylindeno[1,2-c]pyrazole-2(4H)-propanamine, from Example 3C, in 25 ml of MeCN is treated with 1.35 g (0.0139 mole) of MeSO3H dissolved in 5 ml of MeCN. On seeding and rubbing, the crystalline mesylate salt separates; wt., after cooling overnight, 4.1 g (66%); m.p. 151°-153°. Following recrystallization from 20 ml of MeOH-100 ml ether, the cream-colored solid weighs 3.8 g (61%); m.p. 151°-153°.

Workup

  1. temperaturewt., after cooling overnight
  2. customrecrystallization from 20 ml of MeOH-100 ml ether

Sources & evidence

ORD record
ord-46af872ba9904199b1f8219866eb8217
Source dataset
uspto-grants-1979_11
Patent number
US04173634

Reaction notes

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