Triethylamine → 1-Cyclopropanecarbonyl-4-hydroxypiperidine

HRID 374805ノート

反応式

HRID 374805 の反応式
[OH:1][CH:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.C(N(CC)CC)C.[CH:15]1([C:18](Cl)=[O:19])[CH2:17][CH2:16]1>ClCCl>[CH:15]1([C:18]([N:5]2[CH2:6][CH2:7][CH:2]([OH:1])[CH2:3][CH2:4]2)=[O:19])[CH2:17][CH2:16]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 77637Cyclopropanecarbonyl chlorideHCID 79341Piperidin-4-ol

生成物 1

HCID 149949671-Cyclopropanecarbonyl-4-hydroxypiperidine収率 96%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

20 g of 4-hydroxypiperidine was dissolved in 400 ml of dichloromethane, to which 24 g of triethylamine was added. At -60° C., 100 ml of a dichloromethane solution containing 20.7 g of cyclopropanecarbonyl chloride was further added. After completion of the reaction, the reaction solution was extracted with chloroform under salting-out conditions and dried with anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The resultant residue was purified by the use of silica gel column chromatography (elution solvent:dichloroethane), thereby obtaining 32 g of the intended compound (yield 96%).

後処理

  1. additionwas added
  2. additionwas further added
  3. customAfter completion of the reaction
  4. extractionthe reaction solution was extracted with chloroform under salting-out conditions
  5. dry with materialdried with anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe resultant residue was purified by the use of silica gel column chromatography (elution solvent:dichloroethane)

出典と根拠

ORDレコード
ord-4a94089e81ea41c28f26a5919606116b
出典データセット
uspto-grants-1996_01
特許番号
US05482937

反応ノート

読み込み中…