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Hydrochloric Acid → 2-[2-(4-Methylpiperazin-1-yl)ethoxy]-1-(1-naphthyl)ethanol dihydrochloride

HRID 2259368
ノート
印刷プレビュー

反応式

HRID 2259368 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][CH2:9][O:10][CH2:11][CH:12]([C:20]2[C:29]3[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=3)[CH:23]=[CH:22][CH:21]=2)[O:13]C2CCCCO2)[CH2:4][CH2:3]1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1.[OH-].[Na+].[ClH:44]>CC(C)=O.C(OCC)C.C(Cl)(Cl)Cl.O>[ClH:44].[ClH:44].[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][CH2:9][O:10][CH2:11][CH:12]([C:20]2[C:29]3[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=3)[CH:23]=[CH:22][CH:21]=2)[OH:13])[CH2:4][CH2:3]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 521998p-Toluenesulfonic acid monohydrateHCID 536974332-[2-(4-Methylpiperazin-1-yl)ethoxy]-1-(1-naphthyl)-1-(tetrahydropyran-2-yloxy)ethane

生成物 1

HCID 675973272-[2-(4-Methylpiperazin-1-yl)ethoxy]-1-(1-naphthyl)ethanol dihydrochloride

試薬・触媒・溶媒 4

HCID 180
Acetone
溶媒
2 回
HCID 962Water溶媒
HCID 3283Diethyl Ether溶媒
HCID 6212Chloroform溶媒

反応条件

温度
40 °C

実験手順

In 30 ml of acetone was dissolved 3.3 g of 2-[2-(4-methylpiperazin-1-yl)ethoxy]-1-(1-naphthyl)-1-(tetrahydropyran-2-yloxy)ethane. To the solution were added 3.46 g of p-toluenesulfonic acid monohydrate and 7 ml of water at room temperature. The resulting mixture was stirred at the same temperature for 30 minutes and further at 40° C. for 1 hour. The reaction mixture was added to a mixture of 60 ml of chloroform and 60 ml of ice water. The mixture was adjusted to pH 11 with a 10% aqueous sodium hydroxide solution. The organic layer was separated. The aqueous layer was extracted with 20 ml of chloroform. The extract was combined with the previously separated organic layer. The combined organic layer was washed with water and dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure. The residue thus obtained was dissolved in 40 ml of acetone. Hydrogen chloride gas was blown into the solution with ice cooling. The resulting solution was stirred at room temperature for 30 minutes. Thereto was added 40 ml of diethyl ether. The resulting mixture was stirred at the same temperature for 30 minutes. The resulting crystals were collected by filtration, washed with acetone, and dried to obtain 2.35 g of 2-[2-(4-methylpiperazin-1-yl)ethoxy]-1-(1-naphthyl)ethanol dihydrochloride (compound No. 259).

後処理

  1. customThe organic layer was separated
  2. extractionThe aqueous layer was extracted with 20 ml of chloroform
  3. washThe combined organic layer was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was removed by distillation under reduced pressure
  6. customThe residue thus obtained
  7. stirringThe resulting solution was stirred at room temperature for 30 minutes
  8. stirringThe resulting mixture was stirred at the same temperature for 30 minutes
  9. filtrationThe resulting crystals were collected by filtration
  10. washwashed with acetone
  11. customdried

出典と根拠

ORDレコード
ord-c1539199b4cb41a493b8a9428e2b228c
出典データセット
uspto-grants-1995_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05472984

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート