Allylamine → HCID 22181441, 화합물

HRID 1796518노트

반응식

HRID 1796518 반응식
Cl[C:2]1[N:7]=[CH:6][C:5]([C:8]([OH:10])=[O:9])=[CH:4][C:3]=1[N+:11]([O-:13])=[O:12].[CH2:14]([NH2:17])[CH:15]=[CH2:16]>CO>[N+:11]([C:3]1[CH:4]=[C:5]([C:8]([OH:10])=[O:9])[CH:6]=[N:7][C:2]=1[NH:17][CH2:14][CH:15]=[CH2:16])([O-:13])=[O:12]

참가 물질

4

반응물 2

HCID 7853AllylamineHCID 3464596-Chloro-5-nitropyridine-3-carboxylic acid

생성물 1

HCID 22181441HCID 22181441, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 6-chloro-5-nitro-3-pyridinecarboxylic acid (4.72 g, 23.30 mmol) in methanol (70 mL) at room temperature was added allyl amine (5.25 mL, 70.0 mmol) and the mixture was stirred overnight. The reaction was then concentrated in vacuo and the residue taken up into water (100 mL). The solution was brought to pH 3 by addition of 1 M HCl aqueous solution. The resulting suspension was extracted with EtOAc (50 mL). The aqueous phase was back-extracted with additional EtOAc (2×50 mL). The organic phases were combined, dried with MgSO4, and filtered. The solution was concentrated in vacuo providing 5-nitro-6-(2-propenylamino)-3-pyridinecarboxylic acid which was used without further purification.

후처리

  1. concentrationThe reaction was then concentrated in vacuo
  2. additionThe solution was brought to pH 3 by addition of 1 M HCl aqueous solution
  3. extractionThe resulting suspension was extracted with EtOAc (50 mL)
  4. extractionThe aqueous phase was back-extracted with additional EtOAc (2×50 mL)
  5. dry with materialdried with MgSO4
  6. filtrationfiltered
  7. concentrationThe solution was concentrated in vacuo

출처 및 근거

ORD 기록
ord-ee1e2246571d4630b4199e95580a8120
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07030139B2

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