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

HRID 462252

반응식

HRID 462252 반응식
[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

참가 물질

5

반응물 3

HCID 240BenzaldehydeHCID 313Hydrochloric AcidHCID 740491-Methyl-4-piperidone

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c503de4aa7884a33a74ca95625370b3b
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04065617

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