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

Sodium Bisulfate → 3-(4-Bromophenoxy)-6-methoxy-2-(4-methoxyphenyl)benzo[b]thiophene

HRID 632637
노트
인쇄 미리보기

반응식

HRID 632637 반응식
[Br:1][C:2]1[CH:28]=[CH:27][C:5]([O:6][C:7]2[C:8]3[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][C:9]=3[S:10](=O)[C:11]=2[C:12]2[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=2)=[CH:4][CH:3]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3].OS([O-])(=O)=O.[Na+]>C1COCC1>[Br:1][C:2]1[CH:28]=[CH:27][C:5]([O:6][C:7]2[C:8]3[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][C:9]=3[S:10][C:11]=2[C:12]2[CH:13]=[CH:14][C:15]([O:18][CH3:19])=[CH:16][CH:17]=2)=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 516919Sodium BisulfateHCID 21226445Aluminium lithium hydrideHCID 867306513-(4-Bromophenoxy)-6-methoxy-2-(4-methoxyphenyl)benzo[b]thiophene 1-oxide

생성물 1

HCID 867306523-(4-Bromophenoxy)-6-methoxy-2-(4-methoxyphenyl)benzo[b]thiophene수율 91%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
0 °C

실험 절차

A solution of 3-(4-bromophenoxy)-6-methoxy-2-(4-methoxyphenyl)benzo[b]thiophene 1-oxide (970 mg, 2.12 mmol) in THF (5 mL) was cooled to 0° C. To the cooled solution was added LAH (129 mg, 3.39 mmol) in one portion. The reaction mixture was stirred at 0° C. for 30 min after which the mixture was poured into 1 M aq. NaHSO4 solution and extracted with DCM. The organic layer was collected (phase separator) and concentrated in vacuo to afford the crude product which was purified by column chromatography (SiO2, 0-30% EtOAc/Heptane) to afford 3-(4-bromophenoxy)-6-methoxy-2-(4-methoxyphenyl)benzo[b]thiophene (850 mg, 1.93 mmol, 91% yield) as a white solid. 1H NMR (400 MHz, CDCl3) δ ppm=3.83 (s, 3 H), 3.90 (s, 3 H), 6.80-6.99 (m, 5 H), 7.22-7.32 (m, 2 H), 7.32-7.44 (m, 2 H), 7.65 (d, J=9.09 Hz, 2 H).

후처리

  1. extractionextracted with DCM
  2. customThe organic layer was collected (phase separator)
  3. concentrationconcentrated in vacuo
  4. customto afford the crude product which
  5. customwas purified by column chromatography (SiO2, 0-30% EtOAc/Heptane)

출처 및 근거

ORD 기록
ord-ccf74a6d667942b19d7948b5eaaa5acf
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09321746B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트