1-(2,2-Diethoxyethyl)-1'-(4-methoxybenzyl)-1H,1'H-3,4'-bipyrazol-5-amine → HCID 178490761, compound

HRID 1055633

Reaction equation

HRID 1055633 reaction equation
C(O[CH:4](OCC)[CH2:5][N:6]1[C:10]([NH2:11])=[CH:9][C:8]([C:12]2[CH:13]=[N:14][N:15]([CH2:17][C:18]3[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=3)[CH:16]=2)=[N:7]1)C>C(O)C.S(=O)(=O)(O)O>[CH3:25][O:24][C:21]1[CH:22]=[CH:23][C:18]([CH2:17][N:15]2[CH:16]=[C:12]([C:8]3[CH:9]=[C:10]4[NH:11][CH:4]=[CH:5][N:6]4[N:7]=3)[CH:13]=[N:14]2)=[CH:19][CH:20]=1

Participants

4

Reactant 1

HCID 866909601-(2,2-Diethoxyethyl)-1'-(4-methoxybenzyl)-1H,1'H-3,4'-bipyrazol-5-amine

Product 1

HCID 178490761HCID 178490761, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 1118Sulfuric AcidSolvent

Procedure

In a microwave oven (Biotage Initiator, with Dynamic Field Tuning), 155 mg (0.40 mmol) of the compound of Example 2A in 0.4 ml of ethanol and 0.2 ml of 2 M sulphuric acid were heated at 120° C. for 15 min. The reaction was then purified directly by preparative HPLC (Method 11). The product fractions were concentrated and the residue was dried under high vacuum. This gave 54 mg (46% of theory) of the title compound.

Workup

  1. customThe reaction was then purified directly by preparative HPLC (Method 11)
  2. concentrationThe product fractions were concentrated
  3. customthe residue was dried under high vacuum

Sources & evidence

ORD record
ord-f72c1db23d20489c994c6c8744136b83
Source dataset
uspto-grants-2016_07
Patent number
US09394309B2

Linked notes

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