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

HRID 1395467노트

반응식

HRID 1395467 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-4edfe7e2cbfd425f883b105bd6819834
출처 데이터셋
uspto-grants-1980_05
특허 번호
US04203994

반응 노트

불러오는 중…