Hydrochloric Acid → HCID 131710293, compound

HRID 1657693Notes

Reaction equation

HRID 1657693 reaction equation
[CH3:1][N:2]([CH3:30])[CH2:3][CH2:4][CH2:5][N:6]1[CH:10]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:9]2[CH2:17][S:18](=[O:29])(=[O:28])[CH2:19][C:20](=[CH:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[C:8]2=[N:7]1.[ClH:31].CCOCC>C(C(C)=O)C>[ClH:31].[CH3:30][N:2]([CH3:1])[CH2:3][CH2:4][CH2:5][N:6]1[CH:10]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:9]2[CH2:17][S:18](=[O:29])(=[O:28])[CH2:19][C:20](=[CH:21][C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=3)[C:8]2=[N:7]1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 54546254HCID 54546254, compound

Product 1

HCID 131710293HCID 131710293, compound

Reagents, catalysts & solvents 1

HCID 6569Methyl Ethyl KetoneSolvent

Procedure

3a,4,6,7-Tetrahydro-N,N-dimethyl-3-phenyl-7-(phenylmethylene)thiopyrano[4,3-c]pyrazole-2(3H)-propanamine-5,5-dioxide (3.4g) is dissolved in 25ml of warm methyl ethyl ketone, cooled and treated with 1.35ml of 6.1N alcoholic hydrogen chloride. On seeding and rubbing, the crystalline hydrogen chloride salt separates. Ether is added to complete the precipitation and after cooling for about 16 hours the solid is filtered, washed with ether and dried in vacuo to give 3.5g of material, melting point 183°-185°C. Following crystallization from 20ml of methanol-40ml of ether, there remains 2.6g of the title compound, melting point 192°-194°C.

Workup

  1. temperaturecooled
  2. customthe precipitation
  3. temperatureafter cooling for about 16 hours the solid
  4. filtrationis filtered
  5. washwashed with ether
  6. customdried in vacuo

Sources & evidence

ORD record
ord-d4296aace3c74a7b8ce2fb2907defba6
Source dataset
uspto-grants-1976_06
Patent number
US03962222

Reaction notes

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