Allylamine → N-allyl-5-chlorothiophenecarboxamide

HRID 41082

反応式

HRID 41082 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-d34cb3ece78144f5b8c257a05ed29ffc
出典データセット
uspto-grants-2013_09
特許番号
US08530505B2

関連ノート

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