Pentylamine → N-(2-Amino-5-benzyl-6-methylpyrimidine-4-yl)-N-pentylamine

HRID 989707

반응식

HRID 989707 반응식
[CH2:1]([C:8]1[C:9](Cl)=[N:10][C:11]([NH2:15])=[N:12][C:13]=1[CH3:14])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:17]([NH2:22])[CH2:18][CH2:19][CH2:20][CH3:21]>O1CCOCC1>[NH2:15][C:11]1[N:10]=[C:9]([NH:22][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])[C:8]([CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[C:13]([CH3:14])[N:12]=1

참가 물질

4

반응물 2

HCID 8060PentylamineHCID 8202385-Benzyl-4-chloro-6-methylpyrimidin-2-amine

생성물 1

HCID 12043763N-(2-Amino-5-benzyl-6-methylpyrimidine-4-yl)-N-pentylamine수율 89.7%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A mixture of 5-benzyl-4-chloro-6-methylpyrimidine-2-ylamine (500 mg, 2.14 mmol) , amylamine (1.24 ml ) and dioxane (4 ml ) was kept at 95-100° C. for 19 hours. The reaction mixture was concentrated in vacuo, and the residue was extracted with chloroform and a saturated aqueous NaHCO3 solution. The organic layer was washed with saturated brine, dried over sodium sulfate, and concentrated in vacuo. The residue was purified by silica gel column chromatography (2%MeOH/CHCl3) to give the object compound (546 mg, 89.7%).

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. extractionthe residue was extracted with chloroform
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by silica gel column chromatography (2%MeOH/CHCl3)

출처 및 근거

ORD 기록
ord-0c51ed97379a4340923c28e477daca0e
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06458798B1

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