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

HRID 2420124ノート

反応式

HRID 2420124 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-9d17f9327255462783cd98d3afa59506
出典データセット
uspto-grants-1978_08
特許番号
US04109002

反応ノート

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