홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

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

HRID 1198249
노트
인쇄 미리보기

반응식

HRID 1198249 반응식
[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 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

생성물 1

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

시약·촉매·용매 4

HCID 180
Acetone
용매
2회
HCID 962Water용매
HCID 3283Diethyl Ether용매
HCID 6212Chloroform용매

반응 조건

온도
40 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-08f720e1c5cc40a09f5efa8935af240c
출처 데이터셋
uspto-grants-1994_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05280032

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트