Allylamine → N-allyl-5-chlorothiophenecarboxamide

HRID 68470

反応式

HRID 68470 の反応式
[CH2:1]([NH2:4])[CH:2]=[CH2:3].[Cl:5][C:6]1[S:10][C:9]([C:11](Cl)=[O:12])=[CH:8][CH:7]=1>N1C=CC=CC=1.C1COCC1>[CH2:1]([NH:4][C:11]([C:9]1[S:10][C:6]([Cl:5])=[CH:7][CH:8]=1)=[O:12])[CH:2]=[CH2:3]

参加物

5

反応物 2

HCID 7853AllylamineHCID 5892235-Chlorothiophene-2-carbonyl Chloride

生成物 1

HCID 21919842N-allyl-5-chlorothiophenecarboxamide

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

An ice-cooled solution of 2.63 ml (35 mmol) of allylamine in 14.2 ml of absolute pyridine and 14.2 ml of absolute THF is admixed dropwise with 5-chloro-thiophene-2-carbonyl chloride (7.61 g, 42 mmol). Ice-cooling is removed and the mixture is stirred at room temperature for 3 h and then concentrated under reduced pressure. The residue is admixed with water and the solid is filtered off. The crude product is purified by flash chromatography over silica gel (dichloromethane).

後処理

  1. temperatureIce-cooling
  2. customis removed
  3. concentrationconcentrated under reduced pressure
  4. filtrationthe solid is filtered off
  5. customThe crude product is purified by flash chromatography over silica gel (dichloromethane)

出典と根拠

ORDレコード
ord-c02ce5a6e4d64658935876d0d60677c1
出典データセット
uspto-grants-2014_09
特許番号
US08822458B2

関連ノート

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