Hydrochloric Acid → 3-Ethylcarbonyl-5-[(2,4-dichlorophenoxy)methyl]-1,2,4-oxadiazole

HRID 4897

反応式

HRID 4897 の反応式
C(O[C:4]([C:6]1[N:10]=[C:9]([CH2:11][O:12][C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=2[Cl:20])[O:8][N:7]=1)=[O:5])C.[CH2:21]([Mg]Br)[CH3:22].Cl>O1CCCC1>[CH2:21]([C:4]([C:6]1[N:10]=[C:9]([CH2:11][O:12][C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=2[Cl:20])[O:8][N:7]=1)=[O:5])[CH3:22]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 197971323-Ethoxycarbonyl-5-[(2,4-dichlorophenoxy)methyl]-1,2,4-oxadiazoleHCID 178418443HCID 178418443、化合物

生成物 1

HCID 197971233-Ethylcarbonyl-5-[(2,4-dichlorophenoxy)methyl]-1,2,4-oxadiazole収率 83%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-78 °C

実験手順

0.95 g of 3-ethoxycarbonyl-5-[(2,4-dichlorophenoxy)methyl]-1,2,4-oxadiazole was added to 30 ml of tetrahydrofuran. The mixture was cooled to -78° C., and then 3 ml of ethylmagnesium bromide (2M solution) was added dropwise. After the mixture was stirred at -78° C. for 1 hour, it was poured into cold aqueous 5% HCl solution. After the resulted product was extracted with ether and concentrated, it was purified by column chromatography(hexane:ethylacetate=4:1) to obtain 0.75 g of the desired product(yield: 83.0%).

後処理

  1. extractionAfter the resulted product was extracted with ether
  2. concentrationconcentrated
  3. customit was purified by column chromatography(hexane:ethylacetate=4:1)

出典と根拠

ORDレコード
ord-e5bfa70b33c24bb5b62e1dfb336704c5
出典データセット
uspto-grants-1993_09
特許番号
US05242890

関連ノート

読み込み中…