Diethyl Ether → Pyridine-4-amidine hydrochloride

HRID 8595

反応式

HRID 8595 の反応式
[Na].[C:2]([C:4]1[CH:9]=[CH:8][N:7]=[CH:6][CH:5]=1)#[N:3].[Cl-:10].[NH4+:11].C(OCC)C>CO>[ClH:10].[C:2]([C:4]1[CH:9]=[CH:8][N:7]=[CH:6][CH:5]=1)(=[NH:11])[NH2:3]

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 75064-CyanopyridineHCID 25517Ammonium ChlorideHCID 5360545Sodium

生成物 1

HCID 2776844Pyridine-4-amidine hydrochloride収率 93%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of sodium (0.23 g) in methanol (40 ml) was added 4-cyanopyridine (10.62 g) at room temperature. Stirring was continued for 6 h followed by the addition of ammoniumchloride (5.9 g) and stirring was continued for another 10 h. Then diethylether (120 ml) was added and the precipitate was filtered off after 30 min and washed once with diethylether (20 ml). The product was dried under high vacuum. 4-Amidino-pyridine hydrochloride (14.95 g) was obtained as a white powder.

後処理

  1. stirringstirring
  2. waitwas continued for another 10 h
  3. filtrationthe precipitate was filtered off after 30 min
  4. washwashed once with diethylether (20 ml)
  5. customThe product was dried under high vacuum

出典と根拠

ORDレコード
ord-f98f5a335bf343b985a425cce2db865f
出典データセット
uspto-grants-2006_08
特許番号
US07091201B2

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