Formic Acid → HCID 13075532、化合物

HRID 1153969ノート

反応式

HRID 1153969 の反応式
[I:1][C:2](=[C:5]([I:7])[I:6])[CH2:3][OH:4].[CH:8](O)=[O:9]>>[CH:8]([O:4][CH2:3][C:2]([I:1])=[C:5]([I:7])[I:6])=[O:9]

参加物

3

反応物 2

HCID 284Formic AcidHCID 102167312,3,3-Triiodoallyl alcohol

生成物 1

HCID 13075532HCID 13075532、化合物

実験手順

2.0 g of 2,3,3-triiodoallyl alcohol and 30 ml of formic acid were refluxed, with stirring, for 3 hours. After cooling the mixture, the crystals which precipitated were collected by filtration, dissolved in ethyl acetate, adsorbed in a dry silica gel chromatography column and eluted with 3:1 by volume mixture of hexane and ethyl acetate, to give 1.8 g of the desired Compound No. 81 in the form of crystals melting at 84°-85° C.

後処理

  1. temperatureAfter cooling the mixture
  2. customthe crystals which precipitated
  3. filtrationwere collected by filtration
  4. dissolutiondissolved in ethyl acetate
  5. washeluted with 3:1 by volume mixture of hexane and ethyl acetate

出典と根拠

ORDレコード
ord-9967c43190c74e3fbd834ca8706d02c5
出典データセット
uspto-grants-1984_12
特許番号
US04487781

反応ノート

読み込み中…