Triethylamine → 1-Cyclopropanecarbonyl-4-hydroxypiperidine

HRID 1464325노트

반응식

HRID 1464325 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 149949671-Cyclopropanecarbonyl-4-hydroxypiperidine수율 96%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-1da2947e7aaf4281aa0f6e5a67ab5bd7
출처 데이터셋
uspto-grants-1994_04
특허 번호
US05304553

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