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3-Chloro-N,N-dimethyl-1-propanamine → HCID 68129596, 화합물

HRID 1077040
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HRID 1077040 반응식
[Na].[CH2:2]([O:4][C:5]([C:7]1[CH:12]([C:13]2[CH:18]=[CH:17][C:16]([OH:19])=[C:15]([O:20][CH3:21])[CH:14]=2)[C:11]([C:22]([O:24][CH2:25][CH3:26])=[O:23])=[C:10]([CH3:27])[NH:9][C:8]=1[CH3:28])=[O:6])[CH3:3].[CH3:29][N:30]([CH3:35])[CH2:31][CH2:32][CH2:33]Cl>C(O)C>[CH2:2]([O:4][C:5]([C:7]1[CH:12]([C:13]2[CH:18]=[CH:17][C:16]([O:19][CH2:33][CH2:32][CH2:31][N:30]([CH3:35])[CH3:29])=[C:15]([O:20][CH3:21])[CH:14]=2)[C:11]([C:22]([O:24][CH2:25][CH3:26])=[O:23])=[C:10]([CH3:27])[NH:9][C:8]=1[CH3:28])=[O:6])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 669603-Chloro-N,N-dimethyl-1-propanamineHCID 6198691,4-Dihydro-4-(4-hydroxy-3-methoxyphenyl)-2,6-dimethyl-3,5-pyridinedicarboxylic acid diethyl esterHCID 5360545Sodium

생성물 1

HCID 68129596HCID 68129596, 화합물수율 75%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

A solution of 2.3 g of sodium in 100 ml of ethanol is added to a warm solution of 37.5 g of 2,6-dimethyl-4-(3-methoxy-4-hydroxyphenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid diethyl ester (melting point 172°C) in 300 ml of ethanol. The mixture is heated at reflux and 15 g of 3-dimethylaminopropyl chloride are added dropwise. After refluxing for several hours, the mixture is filtered hot, the residue being washed with alcohol, and the filtrate is evaporated in vacuo to yield yellow crystals of melting point 62°C after recrystallization from ligroin-petroleum ether. Yield: 75% of theory.

후처리

  1. temperatureThe mixture is heated
  2. temperatureat reflux
  3. temperatureAfter refluxing for several hours
  4. filtrationthe mixture is filtered hot
  5. washthe residue being washed with alcohol
  6. customthe filtrate is evaporated in vacuo
  7. customto yield yellow crystals of melting point 62°C
  8. customafter recrystallization from ligroin-petroleum ether

출처 및 근거

ORD 기록
ord-1d8c9ed1555644779f5dcb0478cc7d7f
출처 데이터셋
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03959296

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