Methyl iodide → HCID 58484976, compound

HRID 1255434Notes

Reaction equation

HRID 1255434 reaction equation
[H-].[Na+].[Cl:3][C:4]1[N:5]=[CH:6][C:7]2[NH:13][C:12](=[O:14])[C:11]([CH3:16])([CH3:15])[CH2:10][N:9]([C@@H:17]3[CH2:21][CH2:20][C:19]([F:23])([F:22])[CH2:18]3)[C:8]=2[N:24]=1.[CH3:25]I>CC(N(C)C)=O>[Cl:3][C:4]1[N:5]=[CH:6][C:7]2[N:13]([CH3:25])[C:12](=[O:14])[C:11]([CH3:16])([CH3:15])[CH2:10][N:9]([C@@H:17]3[CH2:21][CH2:20][C:19]([F:23])([F:22])[CH2:18]3)[C:8]=2[N:24]=1

Participants

5

Reactant 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 86658720HCID 86658720, compound

Product 1

HCID 58484976HCID 58484976, compound

Reagents, catalysts & solvents 1

HCID 31374DimethylacetamideSolvent

Procedure

60% Sodium hydride in mineral oil (0.210 g, 5.24 mmol) was added to a mixture of (R)-2-chloro-9-(3,3-difluorocyclopentyl)-7,7-dimethyl-8,9-dihydro-5H-pyrimido[4,5-b][1,4]diazepin-6(7H)-one (1.65 g, 4.99 mmol) and methyl iodide (0.34 ml, 5.49 mmol) in dimethylacetamide (18 mL). The reaction mixture was stirred at room temperature for 25 minutes. Ice was added to the reaction mixture and the resultant precipitate collected and rinsed with water. The solid was dried in a pistol in vacuo for 3 hours. The title compound was obtained as a white solid (1.68 g, 98% yield).

Workup

  1. additionIce was added to the reaction mixture
  2. customthe resultant precipitate collected
  3. washrinsed with water
  4. customThe solid was dried in a pistol in vacuo for 3 hours

Sources & evidence

ORD record
ord-c5b71e434b5d401ca34620e92f15bda6
Source dataset
uspto-grants-2013_06
Patent number
US08461149B2

Reaction notes

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