ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Potassium Carbonate → 1-(3-Chlorophenyl)-2-[2-(4-methylpiperazin-1-yl)ethoxy]ethanol dihydrochloride

HRID 362951
ノート
印刷プレビュー

反応式

HRID 362951 の反応式
C([O:4][CH:5]([C:15]1[CH:20]=[CH:19][CH:18]=[C:17]([Cl:21])[CH:16]=1)[CH2:6][O:7][CH2:8][CH2:9]OS(C)(=O)=O)(=O)C.[CH3:22][N:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1.C(=O)([O-])[O-].[K+].[K+].C[O-].[Na+]>CN(C)C=O.O.C(OCC)(=O)C.CO.C(OCC)C>[ClH:21].[ClH:21].[Cl:21][C:17]1[CH:16]=[C:15]([CH:5]([OH:4])[CH2:6][O:7][CH2:8][CH2:9][N:26]2[CH2:27][CH2:28][N:23]([CH3:22])[CH2:24][CH2:25]2)[CH:20]=[CH:19][CH:18]=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

10

反応物 4

HCID 11430Potassium CarbonateHCID 531671-MethylpiperazineHCID 10942334Sodium MethoxideHCID 536841961-Acetoxy-1-(3-chlorophenyl)-2-(2-methanesulfonyloxyethoxy)ethane

生成物 1

HCID 675963491-(3-Chlorophenyl)-2-[2-(4-methylpiperazin-1-yl)ethoxy]ethanol dihydrochloride

試薬・触媒・溶媒 5

HCID 887
Methanol
溶媒
HCID 962Water溶媒
HCID 3283Diethyl Ether溶媒
HCID 6228Dimethylformamide溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

1.40 g of 1-acetoxy-1-(3-chlorophenyl)-2-(2-methanesulfonyloxyethoxy)ethane was dissolved in 7 ml of N,N-dimethylformamide. To the solution were added 0.69 ml of N-methylpiperazine and 1.03 g of potassium carbonate. The mixture was stirred for 3 hours at 80° C. The reaction mixture was cooled and added to a mixture of 30 ml of ice water and 30 ml of diethyl ether. The organic layer was separated. The aqueous layer was extracted with 20 ml of diethyl ether. The extract was combined with the previously separated organic layer. The combined organic layer was washed with water and a saturated aqueous sodium chloride solution in this order, and dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure. The residue thus obtained was mixed with 7 ml of methanol and 45 mg of sodium methoxide. The mixture was allowed to stand overnight at room temperature. The solvent was removed by distillation under reduced pressure. To the residue thus obtained were added 20 ml of ethyl acetate and 10 ml of water. The organic layer was separated. The aqueous layer was extracted with 20 ml of ethyl acetate. The extract was combined with the previously separated organic layer. The combined organic layer was washed with a saturated aqueous sodium chloride solution and then purified by column chromatography (eluant: chloroform/methanol=10/1). To the resulting oily product were added 10 ml of ethanol and 1.2 ml of a 6N dry hydrogen chloride-ethanol solution in this order. To the resulting mixture was added 10 ml of diethyl ether. The mixture was stirred for 30 minutes. The resulting crystals were collected by filtration, washed with a mixture of 2 ml of ethanol and 2 ml of diethyl ether, and dried to obtain 770 mg of 1-(3-chlorophenyl)-2-[2-(4-methylpiperazin-1-yl)ethoxy]ethanol dihydrochloride (compound No. 158).

後処理

  1. temperatureThe reaction mixture was cooled
  2. customThe organic layer was separated
  3. extractionThe aqueous layer was extracted with 20 ml of diethyl ether
  4. washThe combined organic layer was washed with water
  5. dry with materiala saturated aqueous sodium chloride solution in this order, and dried over anhydrous magnesium sulfate
  6. customThe solvent was removed by distillation under reduced pressure
  7. customThe residue thus obtained
  8. waitto stand overnight at room temperature
  9. customThe solvent was removed by distillation under reduced pressure
  10. customTo the residue thus obtained
  11. customThe organic layer was separated
  12. extractionThe aqueous layer was extracted with 20 ml of ethyl acetate
  13. washThe combined organic layer was washed with a saturated aqueous sodium chloride solution
  14. custompurified by column chromatography (eluant: chloroform/methanol=10/1)
  15. additionTo the resulting oily product were added 10 ml of ethanol and 1.2 ml of a 6N dry hydrogen chloride-ethanol solution in this order
  16. additionTo the resulting mixture was added 10 ml of diethyl ether
  17. stirringThe mixture was stirred for 30 minutes
  18. filtrationThe resulting crystals were collected by filtration
  19. washwashed with a mixture of 2 ml of ethanol and 2 ml of diethyl ether
  20. customdried

出典と根拠

ORDレコード
ord-942b311c3b5842a79eb620288c95eebe
出典データセット
uspto-grants-1999_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05872117

反応ノート

読み込み中…

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