4-Aminopyridine → HCID 12822541, 화합물

HRID 127288

반응식

HRID 127288 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1.[C@@H:8]12[C:17](=O)[O:16][C:14](=[O:15])[C@@H:9]1[CH2:10][CH2:11][CH2:12][CH2:13]2.CS(O)(=O)=O>C1(C)C(C)=CC=CC=1>[N:5]1[CH:6]=[CH:7][C:2]([N:1]2[C:14](=[O:15])[CH:9]3[CH:8]([CH2:13][CH2:12][CH2:11][CH2:10]3)[C:17]2=[O:16])=[CH:3][CH:4]=1

참가 물질

5

반응물 3

HCID 17274-AminopyridineHCID 6395Methanesulfonic AcidHCID 641660Hexahydrophthalic anhydride, cis-

생성물 1

HCID 12822541HCID 12822541, 화합물

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

The starting material is prepared as follows: The mixture of 23.5 g of 4- aminopyridine, 38.5 g of cis-1,2-cyclohexanedicarboxylic acid anhydride and 400 ml of xylene is refluxed for 42 hours while stirring and separating the water formed. After the first half-hour, and after 18 hours, 1 ml of methane sulfonic acid is added to the mixture. It is filtered hot, the crystals formed after cooling are filtered off and recrystallized from isopropanol, to yield the 2-(4-pyridyl)-hexahydroisoindole-1,3-dione melting at 165°-168°.

후처리

  1. customThe starting material is prepared
  2. temperatureis refluxed for 42 hours
  3. customseparating the water
  4. customformed
  5. filtrationIt is filtered hot
  6. customthe crystals formed
  7. temperatureafter cooling
  8. filtrationare filtered off
  9. customrecrystallized from isopropanol

출처 및 근거

ORD 기록
ord-aa672faddfbb46fe8114bfc5b5f4b947
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04255429

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