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 4-CHLORO-7-((2-(TRIMETHYLSILYL)ETHOXY)METHYL)-7H-PYRROLO[2,3-D]PYRIMIDINE
941685-26-3

4-CHLORO-7-((2-(TRIMETHYLSILYL)ETHOXY)METHYL)-7H-PYRROLO[2,3-D]PYRIMIDINE synthesis

2synthesis methods
2-(Trimethylsilyl)ethoxymethyl chloride

76513-69-4

4-Chloro-7H-pyrrolo[2,3-d]pyrimidine

3680-69-1

4-CHLORO-7-((2-(TRIMETHYLSILYL)ETHOXY)METHYL)-7H-PYRROLO[2,3-D]PYRIMIDINE

941685-26-3

Sodium hydride (340 mg, 60% dispersed in mineral oil) was added in two portions to a solution of 4-chloropyrrolo[2,3-d]pyrimidine (3a) (1.0 g, 6.5 mmol) in anhydrous DMF (15 mL) under the cooling conditions of an ice-salt bath, keeping the reaction temperature at 0 °C. The reaction temperature was controlled not to exceed 10 °C under nitrogen protection with continuous stirring for 1 hour. Subsequently, 2-(trimethylsilyl)ethoxymethyl chloride (SEMCl) (1.4 g, 8.5 mmol) was slowly added via syringe while ensuring that the temperature did not exceed 10 °C. The reaction mixture was gradually warmed to room temperature and stirring was continued overnight. After completion of the reaction, the reaction was quenched with water, extracted with ethyl acetate (EA) and the organic phase was dried over anhydrous sodium sulfate and concentrated. Purification by preparative fast chromatography (eluent: petroleum ether/ethyl acetate = 19:1) afforded 4-chloro-7-((2-(trimethylsilyl)ethoxy)methyl)-7H-pyrrolo[2,3-d]pyrimidine (3b) (1.834 g, oily product) in 97% yield. Mass spectrum (ESI, m/z): 284 [M + H]+.

76513-69-4 Synthesis
2-(Trimethylsilyl)ethoxymethyl chloride

76513-69-4
367 suppliers
$6.00/1g

3680-69-1 Synthesis
4-Chloro-7H-pyrrolo[2,3-d]pyrimidine

3680-69-1
834 suppliers
$6.00/1g

-

Yield:941685-26-3 100%

Reaction Conditions:

Stage #1: 4-chloro-1H-pyrrolo[2,3-d]pyrimidinewith sodium hydride in N,N-dimethyl-formamide at 20; for 1 h;Cooling with ice;
Stage #2: (2-trimethylethylsilylethoxy)methyl chloride in N,N-dimethyl-formamide;Cooling with ice;

Steps:

1.D Step D: 4-chloro-7-(2-(trimethylsilyl)ethoxy)methyl-7H-pyrrolo[2,3-d]pyrimidine

Under ice-cooling with stirring, 38.4g (250.4mmol, 1.0eq.) 4-chloro-7H-pyrrolo[2,3-d]pyrimidine is dissolved in 200mL dry DMF. 13g (305mmol, 1.2eq) 57% content of NaH was added. The reaction was stirred at room temperature for 1 hour. 50.9g SEMCl was added dropwise under ice-cooling (305mmol, 1.2eq.). After complete addition, the ice bath the reaction was stirred for 1 hour, quenched with water, extracted with ethyl acetate, combined organic phases were washed with brine, dried over sodium sulfate, filtered and concentrated in vacuo, column chromatography on a silica column to give the title compound (71g , yield = 100%).

References:

CN109867676,2019,A Location in patent:Paragraph 0109-0111

4-CHLORO-7-((2-(TRIMETHYLSILYL)ETHOXY)METHYL)-7H-PYRROLO[2,3-D]PYRIMIDINE Related Search:

长子县| 桓台县| 临泉县| 武川县| 百色市| 新野县| 石阡县| 那坡县| 大化| 兴仁县| 财经| 麦盖提县| 淄博市| 墨脱县| 阿合奇县| 保德县| 周口市| 抚松县| 巫溪县| 土默特右旗| 丹阳市| 凤翔县| 牙克石市| 溧阳市| 丽江市| 南靖县| 靖边县| 成武县| 从江县| 西和县| 达尔| 冀州市| 温州市| 洛阳市| 成武县| 水城县| 织金县| 潮州市| 吉木萨尔县| 岳池县| 湘乡市|