Pyridine → HCID 57468510、化合物

HRID 656501ノート

反応式

HRID 656501 の反応式
[C:1]([C:3]1[CH:4]=[CH:5][C:6]([I:12])=[C:7]([CH:11]=1)[C:8]([OH:10])=[O:9])#[N:2].S(Cl)(Cl)=O.[C:17](O)([CH3:20])([CH3:19])[CH3:18].N1C=CC=CC=1>CN(C)C=O.C(Cl)(Cl)Cl>[C:17]([O:9][C:8](=[O:10])[C:7]1[CH:11]=[C:3]([C:1]#[N:2])[CH:4]=[CH:5][C:6]=1[I:12])([CH3:20])([CH3:19])[CH3:18]

参加物

7

反応物 4

HCID 1049PyridineHCID 6386tert-ButanolHCID 24386Thionyl ChlorideHCID 220088225-Cyano-2-iodobenzoic acid

生成物 1

HCID 57468510HCID 57468510、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide触媒HCID 6212Chloroform溶媒

実験手順

8.9 mmol of 5-Cyano-2-iodo-benzoic acid [219841-92-6] is heated at reflux with 6 ml of thionyl-chloride and 1 drop of N,N-dimethylformamide until all the solid dissolves and there is no further gas evolution. The solution is cooled to room temperature and evaporated to dryness. The residue is treated with 32 mmol of dry tert-butyl alcohol and 49 mmol of dry pyridine in 5 ml of chloroform at 0° C. under an Ar atmosphere. After the addition, the mixture is refluxed overnight, cooled, and evaporated to dryness. From the residue the title compound is identified by means of flash chromatography (SiO2 60F) on the basis of the Rf value.

後処理

  1. dissolutiondissolves
  2. customevaporated to dryness
  3. additionAfter the addition
  4. temperaturethe mixture is refluxed overnight
  5. temperaturecooled
  6. customevaporated to dryness

出典と根拠

ORDレコード
ord-94e58acd2a8a423bbb00b04ee58ab219
出典データセット
uspto-grants-2011_12
特許番号
US08071774B2

反応ノート

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