Pyridine → HCID 57468510, 화합물

HRID 656501노트

반응식

HRID 656501 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 57468510HCID 57468510, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide촉매HCID 6212Chloroform용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-94e58acd2a8a423bbb00b04ee58ab219
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08071774B2

반응 노트

불러오는 중…