Methyl iodide → N-(4-Methoxyphenyl)-N-methyl-4-(3-pyridinyl)-2-pyrimidinamine

HRID 2232302ノート

反応式

HRID 2232302 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10]2[N:15]=[C:14]([C:16]3[CH:17]=[N:18][CH:19]=[CH:20][CH:21]=3)[CH:13]=[CH:12][N:11]=2)=[CH:5][CH:4]=1.[H-].[Na+].[CH3:24]I>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([N:9]([CH3:24])[C:10]2[N:15]=[C:14]([C:16]3[CH:17]=[N:18][CH:19]=[CH:20][CH:21]=3)[CH:13]=[CH:12][N:11]=2)=[CH:7][CH:8]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 14346975N-(4-Methoxyphenyl)-4-(pyridin-3-yl)pyrimidin-2-amine

生成物 1

HCID 14722206N-(4-Methoxyphenyl)-N-methyl-4-(3-pyridinyl)-2-pyrimidinamine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

A 2.78 g portion of N-(4-methoxyphenyl)-4-(3-pyridinyl)-2-pyrimidinamine was dissolved in 30 ml of dimethylformamide. A 528 mg portion of sodium hydride (50% in oil) was added, the reaction sealed and stirred for 45 minutes. A solution of 1.70 g of methyl iodide in 2 ml of dimethylformamide was added, the sealed mixture was stirred overnight and the solvent removed. The residue was partitioned between water and chloroform. The organic phase was dried, filtered and evaporated. The residue was crystallized from ether-hexane giving 1.4 g of the desired product as yellow crystals, mp 88°-90° C.

後処理

  1. customthe reaction sealed
  2. stirringthe sealed mixture was stirred overnight
  3. customthe solvent removed
  4. customThe residue was partitioned between water and chloroform
  5. customThe organic phase was dried
  6. filtrationfiltered
  7. customevaporated
  8. customThe residue was crystallized from ether-hexane giving 1.4 g of the desired product as yellow crystals, mp 88°-90° C.

出典と根拠

ORDレコード
ord-2f2344b6e32f4f67b2b3fcb828720e8a
出典データセット
uspto-grants-1988_11
特許番号
US04788195

反応ノート

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