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Pyridine → HCID 21462913, 화합물

HRID 840266
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HRID 840266 반응식
[C:1](Cl)([Cl:3])=[O:2].[NH2:5][C:6]1[CH:7]=[N:8][CH:9]=[CH:10][CH:11]=1.N1C=CC=CC=1>C1(C)C=CC=CC=1.C(Cl)Cl>[ClH:3].[N:8]1[CH:9]=[CH:10][CH:11]=[C:6]([N:5]=[C:1]=[O:2])[CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 1049PyridineHCID 6371PhosgeneHCID 100093-Aminopyridine

생성물 1

HCID 21462913HCID 21462913, 화합물

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

A 1.93 solution of phosgene in toluene (20%) (584 mL) was diluted with dry CH2Cl2 (1 L) and the mixture was stirred at 0° C. under nitrogen atmosphere. A solution of 3-aminopyridine (21.1 grams) and dry pyridine (19 mL) dissolved in dry CH2Cl2 (600 mL) was added dropwise to the stirred solution at 0° C. over a period of 5.5 hours. The mixture was stirred at 0-25° C. for an additional 48 hours. A stream of nitrogen was passed through the solution to remove most of the phosgene and the solution was then evaporated until almost all of the solvent was removed to give the title compound which was then taken up in dry pyridine (850 mL) to give a stock solution of the title compound.

후처리

  1. additionwas added dropwise to the stirred solution at 0° C. over a period of 5.5 hours
  2. stirringThe mixture was stirred at 0-25° C. for an additional 48 hours
  3. customto remove most of the phosgene
  4. customthe solution was then evaporated until almost all of the solvent
  5. customwas removed

출처 및 근거

ORD 기록
ord-25006a80444f4e46ace1ac53934e5c1d
출처 데이터셋
uspto-grants-2002_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06365588B1

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