Dichloromethane → HCID 135702882, compound

HRID 566341Notes

Reaction equation

HRID 566341 reaction equation
[NH2:1][C:2]1[N:6]([CH:7]([CH3:17])[CH2:8][CH2:9][CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:5]=[C:4]([CH2:18][CH3:19])[C:3]=1[C:20]([NH2:22])=[O:21].[CH2:23]1[O:31][C:30]2[CH:29]=[CH:28][C:27]([CH2:32][C:33](OC)=O)=[CH:26][C:25]=2[O:24]1.ClCCl.C(=O)([O-])O.[Na+]>CC(C)([O-])C.[K+]>[CH2:23]1[O:31][C:30]2[CH:29]=[CH:28][C:27]([CH2:32][C:33]3[NH:22][C:20](=[O:21])[C:3]4[C:4]([CH2:18][CH3:19])=[N:5][N:6]([CH:7]([CH3:17])[CH2:8][CH2:9][CH2:10][C:11]5[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=5)[C:2]=4[N:1]=3)=[CH:26][C:25]=2[O:24]1

Participants

6

Reactant 4

HCID 6344DichloromethaneHCID 266588Methyl 2-(1,3-dioxaindan-5-yl)acetateHCID 516892Sodium BicarbonateHCID 21266063HCID 21266063, compound

Product 1

HCID 135702882HCID 135702882, compoundYield 50%

Reagents, catalysts & solvents 1

HCID 23665647Potassium tert-butoxideSolvent

Procedure

19 mg (0.063 mmol) of 5-amino-1-(1-methyl-4-phenyl-butyl)-3-ethyl-1H-pyrazole-4-carboxamide and 35 mg (0.180 mmol) of methyl 3,4-methylenedioxyphenylacetate are refluxed for 6 hours in 0.9 ml of 0.5M ethanolic potassium tert-butoxide solution. After dichloromethane and saturated aqueous sodium hydrogen carbonate solution have been added, the phases are separated. Purification by chromatography gives 14 mg (48%) of a solid, Rf=0.64 (dichloromethane/methanol=15:1).

Workup

  1. customthe phases are separated
  2. customPurification by chromatography

Sources & evidence

ORD record
ord-8b035a99bd384da4b51f3482b1539408
Source dataset
uspto-grants-2001_01
Patent number
US06174884B1

Reaction notes

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