Ammonia → 2-(Methylthio)pyrimidin-4-amine

HRID 16247

反応式

HRID 16247 の反応式
Cl[C:2]1[CH:7]=[CH:6][N:5]=[C:4]([S:8][CH3:9])[N:3]=1.[NH3:10]>CO>[CH3:9][S:8][C:4]1[N:3]=[C:2]([NH2:10])[CH:7]=[CH:6][N:5]=1

参加物

4

反応物 2

HCID 222AmmoniaHCID 971134-Chloro-2-methylthiopyrimidine

生成物 1

HCID 2592252-(Methylthio)pyrimidin-4-amine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 4-chloro-2-methylsulfanylpyrimidine (8 g) and 7N ammonia in methanol (100 mL) at 100° C. was stirred for 2 days in a sealed tube, cooled, concentrated, treated with water, and extracted with ethyl acetate. The extract was washed with brine, dried over anhydrous sodium sulfate, and concentrated. The concentrate was triturated with ethyl ether and filtered. 1H NMR (300 MHz, CDCl3) δ 8.06 (d, 1H), 6.12 (d, 1H), 4.83 (s, 2H), 2.51 (s, 3H).

後処理

  1. temperaturecooled
  2. concentrationconcentrated
  3. additiontreated with water
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated
  8. customThe concentrate was triturated with ethyl ether
  9. filtrationfiltered

出典と根拠

ORDレコード
ord-ee4c67b25ee64efdb3c0893c80b0defa
出典データセット
uspto-grants-2010_06
特許番号
US07737159B2

関連ノート

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