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

HRID 462254

反応式

HRID 462254 の反応式
[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

参加物

5

反応物 3

HCID 240BenzaldehydeHCID 313Hydrochloric AcidHCID 30848514-Piperidone hydrochloride

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2638860426694659ae38256e7d6e47d8
出典データセット
uspto-grants-1977_12
特許番号
US04065617

関連ノート

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