Urea → HCID 67151381、化合物

HRID 2281882ノート

反応式

HRID 2281882 の反応式
N([O-])=O.[Na+].[N:5]1([C:11]([C:13]2[N:18]=[CH:17][C:16](N)=[CH:15][CH:14]=2)=[O:12])[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1.NC(N)=O.[I-:24].[Na+]>Cl>[I:24][C:16]1[CH:15]=[CH:14][C:13]([C:11]([N:5]2[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]2)=[O:12])=[N:18][CH:17]=1

参加物

6

反応物 4

HCID 1176UreaHCID 5238Sodium IodideHCID 23668193Sodium NitriteHCID 671512216-[(Piperidin-1-yl)carbonyl]pyridin-3-amine

生成物 1

HCID 67151381HCID 67151381、化合物収率 23%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

A solution of sodium nitrite (69 g) in concentrated hydrochloric acid (1.5 L) was added to crude 6-(piperidin-1-ylcarbonyl)pyridin-3-amine at 0 C, and the mixture was stirred for 10 minutes. Urea (20 g) was added, and the mixture was stirred for 15 minutes. Sodium iodide (150 g) was added, and the product was separated by filtration and recrystallized from ethanol to give 5-iodo-2-(piperidin-1-ylcarbonyl)pyridine (yield 23% calculated for methyl 5-nitropyridine-2-carboxylate, 71 g).

後処理

  1. stirringthe mixture was stirred for 15 minutes
  2. customthe product was separated by filtration
  3. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-f088320c41864797bec02a9221b498d4
出典データセット
uspto-grants-2015_09
特許番号
US09139587B2

反応ノート

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