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

HRID 2232302노트

반응식

HRID 2232302 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-2f2344b6e32f4f67b2b3fcb828720e8a
출처 데이터셋
uspto-grants-1988_11
특허 번호
US04788195

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