Benzaldehyde → 4-Piperidinone, 1-methyl-3,5-bis(phenylmethylene)-, hydrochloride

HRID 462252

反応式

HRID 462252 の反応式
[CH3:1][N: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.[ClH:17]>C(O)C>[ClH:17].[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][N:2]([CH3:1])[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 740491-Methyl-4-piperidone

生成物 1

HCID 3587084-Piperidinone, 1-methyl-3,5-bis(phenylmethylene)-, hydrochloride

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 57.0 g of 1-methyl-4-piperidone and 106.0 g of benzaldehyde in 400 ml of ethanol is cooled in an ice-bath and treated with hydrogen chloride gas until 250 g is absorbed. The solution is allowed to stand at room temperature for about 16 hours. The resulting solution is seeded, allowed to stand for about 16 hours at room temperature and the crystalline solid filtered on a sintered-glass funnel and washed with cold ethanol and then with ether. After drying in a desiccator, the solid (146 g) is digested in 400 ml of hot ethanol, cooled and filtered to give 120 g of product, melting point 242°-244° C, dec. Recrystallization of 11 g of this material from 35 ml of dimethylformamide gives 9.2 g of product, melting point 242°-244° C, dec.

後処理

  1. customis absorbed
  2. waitto stand for about 16 hours at room temperature
  3. filtrationthe crystalline solid filtered on a sintered-glass funnel
  4. washwashed with cold ethanol
  5. customAfter drying in a desiccator
  6. temperaturecooled
  7. filtrationfiltered

出典と根拠

ORDレコード
ord-c503de4aa7884a33a74ca95625370b3b
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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