4-Aminopyridine → 3-(4-Pyridyl)-3-azaspiro[5,5]undecan-2,4-dione

HRID 127278

反応式

HRID 127278 の反応式
[CH2:1]1[CH2:6][CH2:5][CH2:4][CH2:3][C:2]21[CH2:12][C:11](=[O:13])[O:10][C:8](=O)[CH2:7]2.[NH2:14][C:15]1[CH:20]=[CH:19][N:18]=[CH:17][CH:16]=1.C1(C)C(C)=CC=CC=1>O>[N:18]1[CH:19]=[CH:20][C:15]([N:14]2[C:8](=[O:10])[CH2:7][C:2]3([CH2:1][CH2:6][CH2:5][CH2:4][CH2:3]3)[CH2:12][C:11]2=[O:13])=[CH:16][CH:17]=1

参加物

5

反応物 3

HCID 17274-AminopyridineHCID 7237O-XyleneHCID 27342891,1-Cyclohexanediacetic Anhydride

生成物 1

HCID 128225403-(4-Pyridyl)-3-azaspiro[5,5]undecan-2,4-dione

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The starting material is prepared as follows: The mixture of 25 g of 2,2-cyclohexane diacetic anhydride, 12.92 g of 4-aminopyridine, and 400 ml of xylene is refluxed for 25 hours using a water separator. The hot, supernatant xylene solution is decanted from an oil precipitate (which is discarded), cooled, filtered and the residue recrystallized from ethanol, to yield the 3-(4-pyridyl)-3-azaspiro[5,5]undecan-2,4-dione melting at 213°-215°.

後処理

  1. customThe starting material is prepared
  2. temperatureis refluxed for 25 hours
  3. customThe hot, supernatant xylene solution is decanted from an oil precipitate (which is discarded)
  4. temperaturecooled
  5. filtrationfiltered
  6. customthe residue recrystallized from ethanol

出典と根拠

ORDレコード
ord-9b3b763cada94dab80b9d46af27a0b77
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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