2,3,5-Triiodobenzoic acid → 2,3,5-Triiodobenzoyl chloride

HRID 375030

反応式

HRID 375030 の反応式
[I:1][C:2]1[C:10]([I:11])=[CH:9][C:8]([I:12])=[CH:7][C:3]=1[C:4](O)=[O:5].C(Cl)(=O)C([Cl:16])=O>ClCCl.CN(C=O)C.C1(C)C=CC=CC=1>[I:1][C:2]1[C:10]([I:11])=[CH:9][C:8]([I:12])=[CH:7][C:3]=1[C:4]([Cl:16])=[O:5]

参加物

6

反応物 2

HCID 69482,3,5-Triiodobenzoic acidHCID 65578Oxalyl chloride

生成物 1

HCID 27608062,3,5-Triiodobenzoyl chloride

試薬・触媒・溶媒 3

HCID 6228Dimethylformamide触媒HCID 1140Toluene溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

A mixture of 15.0 g (30.0 mmol) of 2,3,5-triiodobenzoic acid and 19.0 g (150 mmol) of oxalyl chloride in 60 ml of dry dichloromethane was placed under nitrogen and cooled to 0° C. Two drops of dry DMF were added, the ice bath was removed and the resulting suspension was stirred at room temperature for 1.5 hrs. The resulting brown solution was concentrated in vacuo to produce a tan solid. The solid was dissolved in 30 ml of dry toluene and was concentrated in vacuo. The toluene concentration was repeated two more times to yield 2,3,5-triiodobenzoyl chloride as a tan solid.

後処理

  1. customthe ice bath was removed
  2. concentrationThe resulting brown solution was concentrated in vacuo
  3. customto produce a tan solid
  4. concentrationwas concentrated in vacuo
  5. concentrationThe toluene concentration

出典と根拠

ORDレコード
ord-1597f145b8304576ab4ccfc670b2f5fc
出典データセット
uspto-grants-1996_01
特許番号
US05484585

関連ノート

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