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Propylamine → 2-Amino-4-propylamino-6-methylpyrimidine

HRID 54282
ノート
印刷プレビュー

反応式

HRID 54282 の反応式
[NH2:1][C:2]1[N:7]=[C:6](Cl)[CH:5]=[C:4]([CH3:9])[N:3]=1.[CH2:10]([NH2:13])[CH2:11][CH3:12]>C(O)C>[NH2:1][C:2]1[N:7]=[C:6]([NH:13][CH2:10][CH2:11][CH3:12])[CH:5]=[C:4]([CH3:9])[N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 7852Propylamine2 回HCID 218102-Amino-4-chloro-6-methylpyrimidine

生成物 1

HCID 214679952-Amino-4-propylamino-6-methylpyrimidine収率 105.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Under a nitrogen atmosphere, a solution of 17.0 grams (0.12 mole) of 2-amino-4-chloro-6-methylpyrimidine (commercially available) and 20 mL (0.24 mole) of n-propylamine was stirred, and 25 mL of ethanol was added. Upon completion of addition, the reaction mixture was stirred at ambient temperature for one hour. After this time, the reaction mixture was heated to reflux where it stirred for 2.5 hours. An additional five mL of n-propylamine was added to the reaction mixture, then it was allowed to stir at ambient temperature for about 18 hours. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in 250 mL of 10% methanol in methylene chloride. The cloudy solution was filtered through 300 grams of basic alumina (deactivated with 18 mL of water) using 10% methanol in methylene chloride as the eluant. The product-containing fractions were combined and concentrated under reduced pressure, yielding about 21 grams of 2-amino-4-propylamino-6-methylpyrimidine. The NMR spectrum was consistent with the proposed structure.

後処理

  1. additionUpon completion of addition
  2. temperatureAfter this time, the reaction mixture was heated
  3. temperatureto reflux where it
  4. stirringstirred for 2.5 hours
  5. stirringto stir at ambient temperature for about 18 hours
  6. concentrationThe reaction mixture was concentrated under reduced pressure
  7. dissolutionthe residue was dissolved in 250 mL of 10% methanol in methylene chloride
  8. filtrationThe cloudy solution was filtered through 300 grams of basic alumina (deactivated with 18 mL of water)
  9. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-df84997f0aa44d189749d130453906f3
出典データセット
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05622954

反応ノート

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