Benzaldehyde → 4-Piperidinone, 3,5-bis(phenylmethylene)-, hydrochloride

HRID 462254

반응식

HRID 462254 반응식
[ClH:1].[NH:2]1[CH2:7][CH2:6][C:5](=[O:8])[CH2:4][CH2:3]1.[CH:9](=O)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.Cl>C(O)C>[ClH:1].[CH:9](=[C:4]1[C:5](=[O:8])[C:6](=[CH:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:7][NH:2][CH2:3]1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

참가 물질

5

반응물 3

HCID 240BenzaldehydeHCID 313Hydrochloric AcidHCID 30848514-Piperidone hydrochloride

생성물 1

HCID 3557494-Piperidinone, 3,5-bis(phenylmethylene)-, hydrochloride수율 94.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A stirred solution of 10 g of 4-piperidone, hydrochloride, hydrate and 14 g of benzaldehyde in 50 ml of ethanol is cooled to 10° C and treated dropwise with 25 ml of concentrated hydrochloric acid (temperature maintained at less than 25° C during the addition) and refluxed for 4 hours; the product begins to separate soon after refluxing begins. After standing at room temperature for about 16 hours, the resulting solid is filtered, washed with cold ethanol and with ether, and air-dried yielding 19.4 g of material, melting point 272°-274° C, dec.

후처리

  1. temperaturemaintained at less than 25° C during the addition) and
  2. temperaturerefluxed for 4 hours
  3. customto separate soon
  4. temperatureafter refluxing
  5. filtrationthe resulting solid is filtered
  6. washwashed with cold ethanol and with ether
  7. customair-dried

출처 및 근거

ORD 기록
ord-2638860426694659ae38256e7d6e47d8
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04065617

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