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Sodium Methoxide → 2-Methoxy-4-sec. butylamino-5nitro-6-methylpyrimidine

HRID 597466
ノート
印刷プレビュー

反応式

HRID 597466 の反応式
Cl[C:2]1[N:7]=[C:6]([NH:8][CH:9]([CH2:11][CH3:12])[CH3:10])[C:5]([N+:13]([O-:15])=[O:14])=[C:4]([CH3:16])[N:3]=1.[CH3:17][O-:18].[Na+]>CO>[CH3:17][O:18][C:2]1[N:7]=[C:6]([NH:8][CH:9]([CH2:11][CH3:12])[CH3:10])[C:5]([N+:13]([O-:15])=[O:14])=[C:4]([CH3:16])[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 10942334Sodium MethoxideHCID 188014492-Chloro-4-sec. butylamino-5-nitro-6-methylpyrimidine

生成物 1

HCID 214450672-Methoxy-4-sec. butylamino-5nitro-6-methylpyrimidine収率 73.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

17.1 g of 2-chloro-4-sec. butylamino-5-nitro-6-methyl-pyrimidine (0.07 mole) are dissolved in 200 ml of methanol. To this solution is added a solution of 8.1 g of sodium methylate (0.15 mole) in 100 ml of methanol and the mixture is boiled overnight at 100° C bath temperature. After it has been cooled, the solution is evaporated and the resultant red substance is treated with ether and then filtered over Hyflo. The filter residue is washed 5 times with ether and the combined ethereal extracts are then evaporated to yield 12.3 g of 2-methoxy-4-sec. butylamino-5nitro-6-methylpyrimidine which boils at 110° C at 0.001 Torr (=73% yield).

後処理

  1. temperatureAfter it has been cooled
  2. customthe solution is evaporated
  3. additionthe resultant red substance is treated with ether
  4. filtrationfiltered over Hyflo
  5. washThe filter residue is washed 5 times with ether
  6. customthe combined ethereal extracts are then evaporated

出典と根拠

ORDレコード
ord-dccb631b73f543d3b8d59a1c7c4dbf68
出典データセット
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04014677

反応ノート

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