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Allylamine → HCID 22181441、化合物

HRID 1796518
ノート
印刷プレビュー

反応式

HRID 1796518 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 22181441HCID 22181441、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ee1e2246571d4630b4199e95580a8120
出典データセット
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07030139B2

反応ノート

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