1,2-Diphenylethylamine → N-cyano-N'-(1,2-diphenylethyl)-3-pyridinecarboximidamide

HRID 327117

反応式

HRID 327117 の反応式
[C:1]([N:3]=[C:4]([C:9]1[CH:10]=[N:11][CH:12]=[CH:13][CH:14]=1)OC(C)C)#[N:2].[C:15]1([CH:21]([NH2:29])[CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>CO>[C:1]([NH:3][C:4]([C:9]1[CH:10]=[N:11][CH:12]=[CH:13][CH:14]=1)=[N:29][CH:21]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)#[N:2]

参加物

4

反応物 2

HCID 264821,2-DiphenylethylamineHCID 100812013-Pyridinecarboximidic acid, N-cyano-, 1-methylethyl ester

生成物 1

HCID 19734548N-cyano-N'-(1,2-diphenylethyl)-3-pyridinecarboximidamide収率 58%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Isopropyl N-cyano-3-pyridinecarboximidate (0.60 g, 3.2 mmol) was dissolved in methanol (10 ml), and 1,2-diphenylethylamine (0.69 g, 3.5 mmol) was added. The mixture was stirred at room temperature for 45 minutes. After the reaction was completed, the reaction solution was concentrated under reduced pressure. The residual concentrate thus obtained was subjected to chromatography on a silica gel column (WAKO GEL C-200, 50 g) eluting with chloroform-methanol (100:1). The eluted fractions were concentrated under reduced pressure to give N-cyano-N'-(1,2-diphenylethyl)-3 pyridinecarboximidamide (0.60 g, 1.8 mmol, yield: 58%) as colorless syrup. Next, to this syrup was added a 5% hydrogen chloride solution in methanol (2.5 ml). The solution was crystallized from methanol-diethyl ether to give N-cyano-N'-(1,2-diphenylethyl)-3-pyridinecarboximidamide hydrochloride as colorless powder.

後処理

  1. concentrationthe reaction solution was concentrated under reduced pressure
  2. concentrationThe residual concentrate thus
  3. customobtained
  4. washeluting with chloroform-methanol (100:1)
  5. concentrationThe eluted fractions were concentrated under reduced pressure

出典と根拠

ORDレコード
ord-cbb066c65fe94e858d62ddb9d33c4ffa
出典データセット
uspto-grants-1993_12
特許番号
US05272164

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