一二三四区视频,亚洲少妇熟女色,日本久热无码视频网,欧美国产日韩大尺度,亚洲a视频,久久少妇一区二区,日韩999无码视频,刺激久久久久久久,啊啊啊啊不要啊在线

Welcome to chemicalbook!
Chinese English Japanese Germany Korea
010-86108875
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

ChemicalBook CAS DataBase List 5-Azaindole
271-34-1

5-Azaindole synthesis

1synthesis methods
-

Yield:271-34-1 58%

Reaction Conditions:

Stage #1: 6-azaindolewith potassium hydroxide;iodine in N,N-dimethyl-formamide at 20; pH=10; for 1.75 h;
Stage #2: with sodium hydride in tetrahydrofuran at 20; for 0.25 h;
Stage #3: p-toluenesulfonyl chloride in tetrahydrofuran at 20; for 2 h;

Steps:



To a mixture of 6-azaindole (CAS 271-341) (1.72 g) and KOH (2.4 g) in dry DMF(50 ml) under nitrogen was added iodine (3.73 g) portionwise over 15 min. The mixture was stirred at r.t. for a further 90 min and poured into water (600 ml) containing sodium metabisulfite solution (100 ml). Adjusting the solution to pHIO caused the product to precipitate out. The solid was extracted with EtOAc (500 ml). The organic layer was separated, dried over MgSO4, filtered and the solvent removed in vacuo to yield a yellow solid (2.98 g). This solid was dissolved in dry THF (50 ml) and to the mixture was added portionwise NaH (60% dispersion in mineral oil) (630 mg). The mixture was stirred for a further 15 min. Pαrα-toluenesulfonyl chloride (2.42 g) was added in one portion and the mixture stirred at r.t. for 2 hours. The mixture was poured into water (600 ml) and extracted with EtOAc (400 ml). The organic layer was separated, dried over MgSO4, filtered and the solvent removed in vacuo. Purification by column chromatography on silica eluting with 0-10% MeOH/DCM yielded the title compound as a solid (3.37 g, 58%). LCMS 399 [M+H]+, RT 2.99 min. 1H NMR 300 MHz (CDCl3) 8.70 (1H, s), 8.55 (1H, d), 7.90-7.75 (3H, m), 7.70 (1H, s), 7.30 (2H, d), 2.40 (3H, s).

References:

WO2006/38001,2006,A1 Location in patent:Page/Page column 51

5-Azaindole Related Search:

儋州市| 扶风县| 中超| 博野县| 西和县| 潜江市| 河北区| 通渭县| 突泉县| 宿迁市| 西乡县| 乐山市| 灵寿县| 诸城市| 常德市| 察隅县| 乐清市| 建德市| 微山县| 灌阳县| 余姚市| 承德县| 青龙| 阜城县| 高邑县| 行唐县| 元谋县| 阿合奇县| 调兵山市| 土默特左旗| 咸宁市| 涟源市| 上栗县| 咸丰县| 宁阳县| 本溪市| 苗栗县| 砚山县| 广汉市| 黑龙江省| 博客|