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

HRID 375030
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HRID 375030 반응식
[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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

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

생성물 1

HCID 27608062,3,5-Triiodobenzoyl chloride

시약·촉매·용매 3

HCID 6228Dimethylformamide촉매HCID 1140Toluene용매HCID 6344Dichloromethane용매

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이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트
온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1597f145b8304576ab4ccfc670b2f5fc
출처 데이터셋
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05484585

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