Sodium Bicarbonate → HCID 14390540、化合物

HRID 330249ノート

反応式

HRID 330249 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH:15]3[O:17][CH2:16]3)[CH2:10][CH2:9]2)[CH:5]=[CH:6][CH:7]=1.Cl.[NH2:19][CH:20]1[C:28]2[C:23](=[C:24]([CH3:31])[CH:25]=[C:26]([CH3:30])[C:27]=2[OH:29])[CH2:22][C:21]1([CH3:33])[CH3:32].C(=O)(O)[O-].[Na+]>C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[CH2:9][CH2:10][N:11]([CH2:14][CH:15]([OH:17])[CH2:16][NH:19][CH:20]3[C:28]4[C:23](=[C:24]([CH3:31])[CH:25]=[C:26]([CH3:30])[C:27]=4[OH:29])[CH2:22][C:21]3([CH3:33])[CH3:32])[CH2:12][CH2:13]2)[CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 103548864-(3-Chlorophenyl)-1-(2,3-epoxypropyl)piperazineHCID 136041943-Amino-2,2,5,7-tetramethyl-2,3-dihydro-1H-inden-4-ol--hydrogen chloride (1/1)

生成物 1

HCID 14390540HCID 14390540、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

0.21 Gram of 4-(3-chlorophenyl)-1-(2,3epoxypropyl)piperazine was added to a solution containing 0.21 g of 1-amino-2,3-dihydro-7-hydroxy-2,2,4,6-tetra- methyl-1H-indene hydrochloride in 10 ml of ethanol solution, and the mixture was refluxed for 5 hours. After the reaction was completed, the reaction mixture was concentrated by removing the solvent under a reduced pressure, the residue thus obtained was alkalified with 10%-sodium bicarbonate aqueous solution, then extracted with 100 ml of methylene chloride. The extract was washed three times with 100 ml of water each time, then dried with anhydrous magnesium sulfate. The methylene chloride extract was concentrated by removing the solvent under a reduced pressure, and the residue was purified by a silica gel column chromatography (eluent: ethyl acetate : n-hexane=1 : 1) to obtain 0.21 g of 1-{3-[4-(3-chlorophenyl)-1-piperazinyl]-2-hydroxypropylamino}-2,3-dihydro-7-hydroxy-2,2,4,6-tetramethyl-1H-indene.

後処理

  1. temperaturethe mixture was refluxed for 5 hours
  2. concentrationthe reaction mixture was concentrated
  3. customby removing the solvent under a reduced pressure
  4. customthe residue thus obtained
  5. extractionextracted with 100 ml of methylene chloride
  6. washThe extract was washed three times with 100 ml of water each time
  7. dry with materialdried with anhydrous magnesium sulfate
  8. extractionThe methylene chloride extract
  9. concentrationwas concentrated
  10. customby removing the solvent under a reduced pressure
  11. customthe residue was purified by a silica gel column chromatography (eluent: ethyl acetate : n-hexane=1 : 1)

出典と根拠

ORDレコード
ord-30aed1ce291b41e2ba58e5295fc69657
出典データセット
uspto-grants-1990_01
特許番号
US04895847

反応ノート

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