Triethylamine → HCID 39240504、化合物

HRID 551158ノート

反応式

HRID 551158 の反応式
[Cl-].[C:2]([CH:4]1[CH2:9][CH2:8][NH2+:7][CH2:6][CH2:5]1)#[N:3].C(N(CC)CC)C.[CH2:17]([S:19](Cl)(=[O:21])=[O:20])[CH3:18]>ClCCl>[CH2:17]([S:19]([N:7]1[CH2:8][CH2:9][CH:4]([C:2]#[N:3])[CH2:5][CH2:6]1)(=[O:21])=[O:20])[CH3:18]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 11667Ethanesulfonyl chlorideHCID 178510228HCID 178510228、化合物

生成物 1

HCID 39240504HCID 39240504、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

In a dry round bottom flask was placed 4-cyanopiperidinium chloride (13, 5 g, 45.4 mmol) dichloromethane (150 ml) and triethylamine (18.98 ml, 136 mmol). To the reaction was added dropwise ethanesulfonyl chloride (4.56 ml, 45.4 mmol) and the solution stirred 1 hour and quenched with water (100 ml). The mixture was extracted with dichloromethane (3×50 ml) and the combined organic fractions dried (MgSO4), filtered, and the solvent evaporated under reduced pressure. The residue was purified by column chromatography on silica gel, eluting with EtOAc/Hexanes to give 1-(ethylsulfonyl)piperidine-4-carbonitrile (14) as a white solid. MS 203 (M+1)

後処理

  1. customIn a dry round bottom flask was placed
  2. customquenched with water (100 ml)
  3. extractionThe mixture was extracted with dichloromethane (3×50 ml)
  4. dry with materialthe combined organic fractions dried (MgSO4)
  5. filtrationfiltered
  6. customthe solvent evaporated under reduced pressure
  7. customThe residue was purified by column chromatography on silica gel
  8. washeluting with EtOAc/Hexanes

出典と根拠

ORDレコード
ord-be6d3dbf4ae249acba17d0efe653ddbe
出典データセット
uspto-grants-2011_05
特許番号
US07947714B2

反応ノート

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