Dichloromethane methanol → HCID 9885139, compound

HRID 1042385Notes

Reaction equation

HRID 1042385 reaction equation
[CH3:1][C:2]([CH3:31])([CH3:30])[C:3]([N:5]1[CH2:12][C:11]2[C:10]([NH:13][C:14](=[O:22])[C:15]3[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=3)=[N:9][N:8](C(OCC)=O)[C:7]=2[C:6]1([CH3:29])[CH3:28])=[O:4].C(Cl)Cl.CO>CO>[CH3:1][C:2]([CH3:31])([CH3:30])[C:3]([N:5]1[CH2:12][C:11]2[C:10]([NH:13][C:14](=[O:22])[C:15]3[CH:16]=[CH:17][C:18]([F:21])=[CH:19][CH:20]=3)=[N:9][NH:8][C:7]=2[C:6]1([CH3:29])[CH3:28])=[O:4]

Participants

4

Reactant 2

HCID 21226129Dichloromethane methanolHCID 68649346Ethyl 5-(2,2-dimethylpropanoyl)-3-[(4-fluorobenzoyl)amino]-6,6-dimethyl-5,6-dihydropyrrolo[3,4-c]pyrazole-1(4H)-carboxylate

Product 1

HCID 9885139HCID 9885139, compoundYield 86%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

Ethyl 5-(2,2-dimethylpropanoyl)-3-[(4-fluorobenzoyl)amino]-6,6-dimethyl-5,6-dihydropyrrolo[3,4-c]pyrazole-1(4H)-carboxylate (2.0 g, 4.64 mmol) was dissolved in methanol (60 ml), treated with TEA (6.45 ml, 46.4 mmol, 10 eq) and stirred overnight at room temperature. (TLC: CH2Cl2/MeOH 95/5). After evaporation, the solid was treated with diethyl ether/hexane and filtered to afford 1.43 g of the title compound in 86% yield.

Workup

  1. customAfter evaporation
  2. additionthe solid was treated with diethyl ether/hexane
  3. filtrationfiltered

Sources & evidence

ORD record
ord-2827b8c2c9f3474f89bb35b937190710
Source dataset
uspto-grants-2013_10
Patent number
US08557845B2

Reaction notes

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