Methyl iodide → HCID 18538472, compound

HRID 1394356Notes

Reaction equation

HRID 1394356 reaction equation
[C:1]([N:4]1[CH2:9][CH2:8][CH:7]([C:10]([N:12]([C:30]2[CH:35]=[CH:34][CH:33]=[C:32]([Cl:36])[CH:31]=2)[CH2:13][CH2:14][CH2:15][N:16]2[CH2:21][CH2:20][CH:19]([CH2:22][C:23]3[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=3)[CH2:18][CH2:17]2)=[O:11])[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[CH3:37][I:38]>C(#N)C>[I-:38].[C:1]([N:4]1[CH2:5][CH2:6][CH:7]([C:10]([N:12]([CH2:13][CH2:14][CH2:15][N+:16]2([CH3:37])[CH2:17][CH2:18][CH:19]([CH2:22][C:23]3[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=3)[CH2:20][CH2:21]2)[C:30]2[CH:35]=[CH:34][CH:33]=[C:32]([Cl:36])[CH:31]=2)=[O:11])[CH2:8][CH2:9]1)(=[O:3])[CH3:2]

Participants

4

Reactant 2

HCID 6328Methyl iodideHCID 3013681HCID 3013681, compound

Product 1

HCID 18538472HCID 18538472, compoundYield 87%

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

A mixture of the compound obtained in Example 18 (310 mg, 0.60 mmol), methyl iodide (0.75 ml) and acetonitrile (10 ml) was stirred at room temperature for 14 hours. The reaction mixture was concentrated under reduced pressure. To the concentrate was added diethyl ether, and the resulting precipitates were collected by filtration. The precipitates were washed with diethyl ether, and dried under reduced pressure to give the titled compound (344 mg, 0.52 mmol, Yield 87%) as white amorphous substance.

Workup

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionTo the concentrate was added diethyl ether
  3. customthe resulting precipitates
  4. filtrationwere collected by filtration
  5. washThe precipitates were washed with diethyl ether
  6. customdried under reduced pressure

Sources & evidence

ORD record
ord-e163d47a2aee4c0a9457d476acdc602c
Source dataset
uspto-grants-2008_03
Patent number
US07348324B2

Reaction notes

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