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2-(4-Chlorophenyl)ethylamine → HCID 10039554、化合物

HRID 374161
ノート
印刷プレビュー

反応式

HRID 374161 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].[Cl:15][C:16]1[CH:21]=[CH:20][C:19]([CH2:22][CH2:23][NH2:24])=[CH:18][CH:17]=1>CO>[C:1]([NH:3][C:4]([C:9]1[CH:10]=[N:11][CH:12]=[CH:13][CH:14]=1)=[N:24][CH2:23][CH2:22][C:19]1[CH:20]=[CH:21][C:16]([Cl:15])=[CH:17][CH:18]=1)#[N:2]
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 674302-(4-Chlorophenyl)ethylamineHCID 100812013-Pyridinecarboximidic acid, N-cyano-, 1-methylethyl ester

生成物 1

HCID 10039554HCID 10039554、化合物収率 79%

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 2-(4-chlorophenyl)ethylamine (0.55 g, 3.5 mmol) was added. The mixture was stirred at room temperature for 2.5 hours. After the reaction was completed, the reaction solution was concentrated under reduced pressure. The residual concentrate 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, and the concentrated residue thus obtained was further crystallized from methanol-diethyl ether to give the title compound (0.71 g, 2.5 mmol, yield: 79%) as colorless powder.

後処理

  1. concentrationthe reaction solution was concentrated under reduced pressure
  2. concentrationThe residual concentrate
  3. washeluting with chloroform-methanol (100:1)
  4. concentrationThe eluted fractions were concentrated under reduced pressure
  5. customthe concentrated residue thus obtained
  6. customwas further crystallized from methanol-diethyl ether

出典と根拠

ORDレコード
ord-bafd0f783850469db5ab5757efbaec15
出典データセット
uspto-grants-1992_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05166347

反応ノート

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