Hydrochloric Acid → HCID 67009100, compound

HRID 1472210Notes

Reaction equation

HRID 1472210 reaction equation
[ClH:1].[CH3:2][CH2:3][O:4][C:5]([N:7]1[C:11]([NH:12][C:13](=[O:30])[C:14]2[CH:19]=[CH:18][C:17]([N:20]3[CH2:25][CH2:24][N:23]([CH3:26])[CH2:22][CH2:21]3)=[CH:16][C:15]=2[N+:27]([O-:29])=[O:28])=[C:10]2[CH2:31][N:32](C(OC(C)(C)C)=O)[C:33]([CH3:35])([CH3:34])[C:9]2=[N:8]1)=[O:6]>O1CCOCC1>[ClH:1].[ClH:1].[CH2:3]([O:4][C:5]([N:7]1[C:11]([NH:12][C:13](=[O:30])[C:14]2[CH:19]=[CH:18][C:17]([N:20]3[CH2:25][CH2:24][N:23]([CH3:26])[CH2:22][CH2:21]3)=[CH:16][C:15]=2[N+:27]([O-:29])=[O:28])=[C:10]2[CH2:31][NH:32][C:33]([CH3:34])([CH3:35])[C:9]2=[N:8]1)=[O:6])[CH3:2]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 57703913HCID 57703913, compound

Product 1

HCID 67009100HCID 67009100, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Procedure

A solution of 4N HCl in 1,4-dioxane (4 eq., 18.4 mL, 73.6 mmol) was added to a stirred solution of 6,6-dimethyl-3-[4-(4-methyl-piperazin-1-yl)-2-nitro-benzoylamino]-4H,6H-pyrrolo[3,4-c]pyrazole-2,5-dicarboxylic acid 5-tert-butyl ester 2-ethyl ester (10.5 g, 18.4 mmol) in 1,4-dioxane (100 mL) at room temperature. Stirring was continued for 30 hours. After removal of the solvent, the crude material was treated with diethyl ether (2×100 mL) and evaporated to dryness. The title compound was obtained after crystallization from diethyl ether as yellow solid (10 g, quantitative).

Workup

  1. customAfter removal of the solvent
  2. additionthe crude material was treated with diethyl ether (2×100 mL)
  3. customevaporated to dryness

Sources & evidence

ORD record
ord-d3f0ea5e13d34718ad5d70d59e2a18bd
Source dataset
uspto-grants-2015_04
Patent number
US09012487B2

Reaction notes

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