Triethylamine → 2-Nitro-5-(4-acetylamino-1-piperidyl)benzaldehyde dimethylacetal

HRID 477178

反応式

HRID 477178 の反応式
[CH3:1][O:2][CH:3]([O:14][CH3:15])[C:4]1[CH:9]=[C:8](Cl)[CH:7]=[CH:6][C:5]=1[N+:11]([O-:13])=[O:12].Cl.[C:17]([NH:20][CH:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1)(=[O:19])[CH3:18].C(=O)([O-])[O-].[Na+].[Na+].C(N(CC)CC)C>CN1CCCC1=O.C(OCC)C>[CH3:1][O:2][CH:3]([O:14][CH3:15])[C:4]1[CH:9]=[C:8]([N:24]2[CH2:25][CH2:26][CH:21]([NH:20][C:17](=[O:19])[CH3:18])[CH2:22][CH2:23]2)[CH:7]=[CH:6][C:5]=1[N+:11]([O-:13])=[O:12]

参加物

7

反応物 4

HCID 8471TriethylamineHCID 10340Sodium CarbonateHCID 35700934-Chloro-2-(dimethoxymethyl)-1-nitrobenzeneHCID 114011054-Acetamidopiperidine dihydrochloride

生成物 1

HCID 190868632-Nitro-5-(4-acetylamino-1-piperidyl)benzaldehyde dimethylacetal

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
120 °C

実験手順

12 Grams of 2-nitro-5-chlorobenzaldehyde dimethyl acetal, 16.3 g of 4-acetylaminopiperidine hydrochloride, 13.7 g of sodium carbonate and 13 ml of triethylamine in 150 ml of N-methylpyrrolidone solution were mixed together and reacted by heating at 120° C. for 12 hours with stirring under nitrogen gas stream. After the reaction was completed, the solvent was removed by evaporation and thus obtained residue was added with water and extracted with dichloromethane, then the extract was washed with water and with an aqueous solution saturated with sodium chloride, then dried with anhydrous sodium sulfate. The solvent was removed by evaporation and the residue thus obtained was added with diethyl ether, then the crystals formed were collected by filtration to yield 11.2 g of 2-nitro-5-(4-acetylamino-1-piperidyl)benzaldehyde dimethylacetal.

後処理

  1. customreacted
  2. customthe solvent was removed by evaporation and thus obtained residue
  3. additionwas added with water
  4. extractionextracted with dichloromethane
  5. washthe extract was washed with water and with an aqueous solution saturated with sodium chloride
  6. dry with materialdried with anhydrous sodium sulfate
  7. customThe solvent was removed by evaporation
  8. customthe residue thus obtained
  9. customthe crystals formed
  10. filtrationwere collected by filtration

出典と根拠

ORDレコード
ord-67b3db273b304161b3597310c64abb49
出典データセット
uspto-grants-1989_12
特許番号
US04886809

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