4-Toluenesulfonyl chloride → HCID 86696633、化合物

HRID 1468613ノート

反応式

HRID 1468613 の反応式
[NH2:1][N:2]1[C:10]2[C:6]([N:7]3[N:13]([CH3:14])[C:12](=[O:15])[N:11]([CH2:16][CH2:17][OH:18])[CH:8]3[N:9]=2)=[C:5]([C:19]2[O:20][CH:21]=[CH:22][CH:23]=2)[N:4]=[CH:3]1.[C:24]1([CH3:34])[CH:29]=[CH:28][C:27]([S:30](Cl)(=[O:32])=[O:31])=[CH:26][CH:25]=1.CCCCCC>N1C=CC=CC=1>[CH3:34][C:24]1[CH:29]=[CH:28][C:27]([S:30]([O:18][CH2:17][CH2:16][N:11]2[CH:8]3[N:9]=[C:10]4[C:6]([N:7]3[N:13]([CH3:14])[C:12]2=[O:15])=[C:5]([C:19]2[O:20][CH:21]=[CH:22][CH:23]=2)[N:4]=[CH:3][N:2]4[NH2:1])(=[O:32])=[O:31])=[CH:26][CH:25]=1

参加物

5

反応物 3

HCID 73974-Toluenesulfonyl chlorideHCID 8058HexaneHCID 66826349HCID 66826349、化合物

生成物 1

HCID 86696633HCID 86696633、化合物収率 79.1%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
26 °C

実験手順

A mixture of 5-amino-8-(2-furyl)-3-(2-hydroxyethyl)-1-methyl-[1,2,4]triazolo[5,1-f]purin-2-one obtained in step 6 (3.5 g, 11 mmol), p-toluene sulphonylchloride (5.2 g, 27 mmol) were taken in pyridine (30 ml) and stirred at 25-27° C. for 16 hours. To the reaction mixture hexane (100 ml) was added and solid obtained was filtered off and washed with water (100 ml) followed by hexane (100 ml) to obtain 2-[5-amino-8-(2-furyl)-1-methyl-2-oxo-[1,2,4]triazolo[5,1-f]purin-3-yl]ethyl 4-methylbenzenesulfonate (4.1 g, 78%) as a brown solid.

後処理

  1. customsolid obtained
  2. filtrationwas filtered off
  3. washwashed with water (100 ml)

出典と根拠

ORDレコード
ord-f1807427e03142fe8bca9e4000597602
出典データセット
uspto-grants-2015_04
特許番号
US09006177B2

反応ノート

読み込み中…