반응 #725903
ord-79436a047415479ca8505657f7179884
반응 방정식
[4-(2-Hydroxy-ethoxycarbonylamino)-phenoxy]-acetic acid methyl ester
(4-Isocyanato-phenoxy)-acetic acid methyl ester
→
30
수율 56.5%
{4-[2-(4-Methoxycarbonylmethoxy-phenylcarbamoyloxy)-ethoxycarbonylamino]-phenoxy}-acetic acid methyl ester
수율 56.5%
반응물
시약
없음
용매
반응 조건
온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1workup.DISTILLATIONToluene was distilled off
- 2workup.ADDITIONwater (10 ml) was added
- 3추출Crude 30 was extracted into chloroform
- 4건조dried over sodium sulphate
- 5workup.DISTILLATIONdistilled
- 6기타purified by column chromatography on silica gel
실험 절차
To [4-(2-Hydroxy-ethoxycarbonylamino)-phenoxy]-acetic acid methyl ester 29 (1 g, 3.72 mmol) in toluene (10 ml) was added (4-Isocyanato-phenoxy)-acetic acid methyl ester 28 (0.8 g, 3.8 mmol) at room temperature and heated to 50° C. for 20 hours. Toluene was distilled off and water (10 ml) was added. Crude 30 was extracted into chloroform, dried over sodium sulphate, distilled and purified by column chromatography on silica gel using chloroform as eluant to get pure 30 (1 g, 56.5%) as a white fluffy powder.