4-Toluenesulfonyl chloride → HCID 86696633, 화합물

HRID 1468613노트

반응식

HRID 1468613 반응식
[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

참가 물질

5

반응물 3

HCID 73974-Toluenesulfonyl chlorideHCID 8058HexaneHCID 66826349HCID 66826349, 화합물

생성물 1

HCID 86696633HCID 86696633, 화합물수율 79.1%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
26 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-f1807427e03142fe8bca9e4000597602
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09006177B2

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