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

HRID 460440

反応式

HRID 460440 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-d0f51b1d18cf40e7b1cd4b0b3fd62358
出典データセット
uspto-grants-2007_03
特許番号
US07196200B2

関連ノート

読み込み中…