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

Hexane → 5-Chloro-3-hydroxy-3-(2-methoxy-4-triisopropylsilanyloxyphenyl)-1,3-dihydroindol-2-one

HRID 2361843
노트
인쇄 미리보기

반응식

HRID 2361843 반응식
C([Li])CCC.CCCCCC.Br[C:13]1[CH:29]=[CH:28][C:16]([O:17][Si:18]([CH:25]([CH3:27])[CH3:26])([CH:22]([CH3:24])[CH3:23])[CH:19]([CH3:21])[CH3:20])=[CH:15][C:14]=1[O:30][CH3:31].[Na].[Cl:33][C:34]1[CH:35]=[C:36]2[C:40](=[CH:41][CH:42]=1)[NH:39][C:38](=[O:43])[C:37]2=[O:44].ClC1C=C2C(=CC=1)NC(=O)C2=O.[H-].[Na+].[Cl-].[NH4+]>C1COCC1>[Cl:33][C:34]1[CH:35]=[C:36]2[C:40](=[CH:41][CH:42]=1)[NH:39][C:38](=[O:43])[C:37]2([OH:44])[C:13]1[CH:29]=[CH:28][C:16]([O:17][Si:18]([CH:25]([CH3:27])[CH3:26])([CH:22]([CH3:24])[CH3:23])[CH:19]([CH3:21])[CH3:20])=[CH:15][C:14]=1[O:30][CH3:31]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 7

HCID 8058HexaneHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 872035-chloro-1H-indole-2,3-dioneHCID 11314363(4-Bromo-3-methoxyphenoxy)triisopropylsilaneHCID 670430655-Chlorisatin sodium saltHCID 178418339Butyllithium

생성물

1
HCID 670433315-Chloro-3-hydroxy-3-(2-methoxy-4-triisopropylsilanyloxyphenyl)-1,3-dihydroindol-2-one수율 41%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of n-butyllithium in hexane (1.6 m, 19.6 ml, 31.4 mmol) was slowly added dropwise to a solution of (4-bromo-3-methoxyphenoxy)triisopropylsilane (8.67 g, 24.1 mmol) in THF (100 ml) at −15° C. After 15 min, a solution of 5-chloroisatin sodium salt [prepared by treating a solution of 5-chloroisatin (3.65 g, 20.1 mmol) in THF with one equivalent of sodium hydride at 0° C. for one h] was added dropwise to the solution of the organolithium species. The reaction mixture was allowed to warm to room temperature and was stirred for a further hour. Aqueous ammonium chloride solution was added to the reaction solution while stirring, and the mixture was extracted with ethyl acetate. The combined organic phase was washed with water and saturated sodium chloride solution, dried over magnesium sulfate and concentrated under reduced pressure. Purification by chromatography on silica gel (mobile phase 10-30% gradient of ethyl acetate in dichloromethane) afforded 3.8 g (41%) of the desired adduct.

후처리

  1. stirringwhile stirring
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe combined organic phase was washed with water and saturated sodium chloride solution
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customPurification by chromatography on silica gel (mobile phase 10-30% gradient of ethyl acetate in dichloromethane)

출처 및 근거

ORD 기록
ord-178f3fa3525c4ee6bed1e5437b2065b0
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08691815B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트