Methyl iodide → HCID 68896686, compound

HRID 1765361Notes

Reaction equation

HRID 1765361 reaction equation
C(OC([N:8]([C:26]1[CH:30]=[C:29]([CH3:31])[N:28](C(OC(C)(C)C)=O)[N:27]=1)[C:9]1[C:18]2[C:13](=[CH:14][C:15](C(O)=O)=[CH:16][CH:17]=2)[C:12](=[O:22])[N:11]([CH:23]([CH3:25])[CH3:24])[N:10]=1)=O)(C)(C)C.[C:39]([O-:42])([O-])=[O:40].[K+].[K+].[CH3:45]I>ClCCl>[CH3:45][O:42][C:39]([C:15]1[CH:14]=[C:13]2[C:18](=[CH:17][CH:16]=1)[C:9]([NH:8][C:26]1[CH:30]=[C:29]([CH3:31])[NH:28][N:27]=1)=[N:10][N:11]([CH:23]([CH3:25])[CH3:24])[C:12]2=[O:22])=[O:40]

Participants

5

Reactant 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 21106512HCID 21106512, compound

Product 1

HCID 68896686HCID 68896686, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

1-[tert-Butoxycarbonyl-(1-tert-butoxycarbonyl-5-methyl-1H-pyrazol-3-yl)-amino]-3-isopropyl-4-oxo-3,4-dihydro-phthalazine-6-carboxylic acid (10 mg, 0.019 mmol) (Intermediate of Example M-1) was dissolved in dichloromethane (DCM) (1 ml). To this was added K2CO3 (3.1 mg, 0.028 mmol) followed by methyl iodide (3.3 mg, 0.028 mmol) and the reaction mixture was stirred at room temperature for 30 minutes. After this time the reaction mixture was partitioned between ethyl acetate (10 ml) and water (10 ml). The organic layer was separated, dried (MgSO4), filtered and concentrated under vacuum.

Workup

  1. customAfter this time the reaction mixture was partitioned between ethyl acetate (10 ml) and water (10 ml)
  2. customThe organic layer was separated
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated under vacuum

Sources & evidence

ORD record
ord-3ec8906f6fc34aeaac7c97295ebe78bb
Source dataset
uspto-grants-2007_06
Patent number
US07226923B2

Reaction notes

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