Ethyl chloroformate → [(3-Phenyl-5-isoxazolyl)methyl]carbamic acid, ethyl ester

HRID 2420124노트

반응식

HRID 2420124 반응식
[NH2:1][CH2:2][C:3]1[O:7][N:6]=[C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:4]=1.Cl[C:15]([O:17][CH2:18][CH3:19])=[O:16]>N1C=CC=CC=1>[C:8]1([C:5]2[CH:4]=[C:3]([CH2:2][NH:1][C:15](=[O:16])[O:17][CH2:18][CH3:19])[O:7][N:6]=2)[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

참가 물질

4

반응물 2

HCID 10928Ethyl chloroformateHCID 27641651-(3-Phenyl-1,2-oxazol-5-yl)methanamine

생성물 1

HCID 60025831[(3-Phenyl-5-isoxazolyl)methyl]carbamic acid, ethyl ester

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A 7 g. portion of the product of Example 8 was dissolved in 50 ml. of pyridine, cooled in an ice bath, and combined with 10 ml. of ethyl chloroformate. The mixture was stirred at ice bath temperature for 1 hour and allowed to warm to room temperature while being stirred for 2 hours more. The mixture was then poured into ice water and the crude product was separated by filtration and purified by chromatography over silica gel with ethyl acetate as the eluent. The yield was 6 g. of purified [(3-phenyl-5-isoxazolyl)-methyl]carbamic acid, ethyl ester, m.p. 82°.

후처리

  1. stirringwhile being stirred for 2 hours more
  2. customthe crude product was separated by filtration
  3. custompurified by chromatography over silica gel with ethyl acetate as the eluent

출처 및 근거

ORD 기록
ord-9d17f9327255462783cd98d3afa59506
출처 데이터셋
uspto-grants-1978_08
특허 번호
US04109002

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