Urea → HCID 67151381, 화합물

HRID 2064238노트

반응식

HRID 2064238 반응식
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

참가 물질

6

반응물 4

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

생성물 1

HCID 67151381HCID 67151381, 화합물수율 23%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-5d7cfa3f9f034f9d8d8f3bf21c39f1a2
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08288405B2

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