반응 #601405

반응 방정식

2,4,6-trimethylphenol

Triphosgene

pyridine

→

mesityl chloroformate

용매

CH2Cl2

CH2Cl2

반응 조건

후처리

1. 1
   workup.ADDITIONadded dropwise
2. 2
   온도to warm to 25° C. over 18 h, at which
3. 3
   기타was quenched with 10 mL 1 normal (N) hydrochloric acid (HCl; aq)
4. 4
   추출extracted with EtOAc
5. 5
   세척The organic layer was washed with 1 N HCl (aq)
6. 6
   건조dried over Na2SO4
7. 7
   농축concentrated

실험 절차

2,4,6-trimethylphenol (272 mg, 2.00 mmol, 1.0 equiv) was dissolved in CH2Cl2 (3.33 mL, 0.3 M) under nitrogen (N2) and cooled to 0° C. Triphosgene (208 mg, 0.700 mmol, 0.35 equiv) was dissolved in CH2Cl2 (3.33 mL) and added dropwise, followed by pyridine (0.162 mL, 2.00 mmol, 1.0 equiv). The mixture was allowed to warm to 25° C. over 18 h, at which point the reaction was quenched with 10 mL 1 normal (N) hydrochloric acid (HCl; aq) and extracted with EtOAc. The organic layer was washed with 1 N HCl (aq), dried over Na2SO4, and concentrated to give mesityl chloroformate as an oil (88% purity by 1H NMR spectroscopy). The chloroformate so prepared was used directly in the next step without further purification.

출처