Propionyl chloride → 3-(N-propionyl-N-n-propylamino)chroman

HRID 266165ノート

反応式

HRID 266165 の反応式
[C:1](Cl)(=[O:4])[CH2:2][CH3:3].[CH2:6]([NH:9][CH:10]1[CH2:19][C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[O:12][CH2:11]1)[CH2:7][CH3:8]>C(Cl)Cl.[OH-].[Na+]>[C:1]([N:9]([CH:10]1[CH2:19][C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[O:12][CH2:11]1)[CH2:6][CH2:7][CH3:8])(=[O:4])[CH2:2][CH3:3]

参加物

5

反応物 2

HCID 62324Propionyl chlorideHCID 195921083-(N-n-propylamino)chroman

生成物 1

HCID 108481013-(N-propionyl-N-n-propylamino)chroman収率 62%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

Propionyl chloride (2.8 g, 29 mmol) was added to a mixture of 15 (1.2 g, 6.4 mmol) in CH2Cl2 and 5% aqueous NaOH. The mixture was stirred for 30 min and separated. The organic layer was extracted with water, separated and dried (MgSO4). The crude product was chromatographed (SiO2) with light petroleum-ether (2:1) as eluant yielding 0.98 g (62%) of 3-(N-propionyl-N-n-propylamino)chroman (16).

後処理

  1. customseparated
  2. extractionThe organic layer was extracted with water
  3. customseparated
  4. dry with materialdried (MgSO4)
  5. customThe crude product was chromatographed (SiO2) with light petroleum-ether (2:1) as eluant

出典と根拠

ORDレコード
ord-2e0385becbd147b898d3b6c0314d7ab3
出典データセット
uspto-grants-1997_07
特許番号
US05650427

反応ノート

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