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

Sodium Hydroxide → 1-[(5-Chloroindol-2-yl)sulfonyl]-3-(ethyl)piperazine

HRID 352800
노트
인쇄 미리보기

반응식

HRID 352800 반응식
[OH-].[Na+].O1CCOCC1.[Cl:9][C:10]1[CH:11]=[C:12]2[C:16](=[CH:17][CH:18]=1)[N:15](S(C1C=CC=CC=1)(=O)=O)[C:14]([S:28]([N:31]1[CH2:36][CH2:35][NH:34][CH:33]([CH2:37][CH3:38])[CH2:32]1)(=[O:30])=[O:29])=[CH:13]2.[Cl-].[NH4+]>C(OCC)(=O)C.O>[Cl:9][C:10]1[CH:11]=[C:12]2[C:16](=[CH:17][CH:18]=1)[NH:15][C:14]([S:28]([N:31]1[CH2:36][CH2:35][NH:34][CH:33]([CH2:37][CH3:38])[CH2:32]1)(=[O:30])=[O:29])=[CH:13]2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 14798Sodium HydroxideHCID 25517Ammonium ChlorideHCID 312751,4-DioxaneHCID 22710634HCID 22710634, 화합물

생성물 1

HCID 227098481-[(5-Chloroindol-2-yl)sulfonyl]-3-(ethyl)piperazine

시약·촉매·용매 2

HCID 962Water용매
HCID 8857
Ethyl Acetate
용매

반응 조건

온도
80 °C

실험 절차

A 1N aqueous solution (16 ml) of sodium hydroxide was added to a 1,4-dioxane solution (200 ml) of 1-[(5-chloro-1-phenylsulfonylindol-2-yl)sulfonyl]-3-(ethyl)piperazine (3.78 g) and the resulting mixture was stirred at 80° C. for 11.5 hours. A saturated aqueous solution of ammonium chloride was added to the reaction mixture. Distilled water and ethyl acetate were then added and the water layer was extracted three time. The organic layers were combined, dried over anhydrous magnesium sulfate and distilled under reduced pressure to remove the solvent. The residue was subjected to chromatography on a silica gel column (methanol:methylene chloride=1:100), followed by crystallization from tetrahydrofuran—diethyl ether, whereby the title compound (2.54 g) was obtained as needle crystals.

후처리

  1. extractionthe water layer was extracted three time
  2. dry with materialdried over anhydrous magnesium sulfate
  3. distillationdistilled under reduced pressure
  4. customto remove the solvent
  5. customfollowed by crystallization from tetrahydrofuran—diethyl ether, whereby the title compound (2.54 g)
  6. customwas obtained as needle crystals

출처 및 근거

ORD 기록
ord-405cd9d5df7248f09349e6d88a6a9ea3
출처 데이터셋
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06747023B1

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트