4-Aminopyridine → HCID 12822541、化合物

HRID 127288

反応式

HRID 127288 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 12822541HCID 12822541、化合物

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-aa672faddfbb46fe8114bfc5b5f4b947
出典データセット
uspto-grants-1981_03
特許番号
US04255429

関連ノート

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