Sodium Thiosulfate → 4-(2-Butynyloxy)-6-methanesulfonylpyrimidine

HRID 1592244ノート

反応式

HRID 1592244 の反応式
[CH2:1]([O:5][C:6]1[CH:11]=[C:10](SC)[N:9]=[CH:8][N:7]=1)[C:2]#[C:3][CH3:4].Cl[C:15]1C=CC=C(C(OO)=O)C=1.[S:25]([O-:29])([O-])(=[O:27])=S.[Na+].[Na+]>C(Cl)(Cl)Cl>[CH2:1]([O:5][C:6]1[CH:11]=[C:10]([S:25]([CH3:15])(=[O:29])=[O:27])[N:9]=[CH:8][N:7]=1)[C:2]#[C:3][CH3:4]

参加物

5

反応物 3

HCID 24477Sodium ThiosulfateHCID 70297m-Chloroperbenzoic acidHCID 225998774-(2-Butynyloxy)-6-methylthiopyrimidine

生成物 1

HCID 225998634-(2-Butynyloxy)-6-methanesulfonylpyrimidine

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
0 °C

実験手順

To 14 ml of chloroform were added 4-(2-butynyloxy)-6-methylthiopyrimidine and 3.5 g of m-chloroperbenzoic acid (>65%), followed by stirring at 0° C. for 10 hours. The reaction mixture was then poured into a saturated aqueous sodium thiosulfate solution and extracted three times with chloroform. The chloroform layers were combined, washed with water, dried over anhydrous magnesium sulfate, and then concentrated. The residue was subjected to silica gel column chromatography to give 1.4 g of 4-(2-butynyloxy)-6-methanesulfonylpyrimidine.

後処理

  1. extractionextracted three times with chloroform
  2. washwashed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-f3a961b0cac748c6adc58b759eb1d938
出典データセット
uspto-grants-2007_11
特許番号
US07291730B2

反応ノート

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