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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

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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:

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