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

Bromine → 4-bromo-5,6,7,8-tetrahydro-1(2H)-Isoquinolinone

HRID 1713397
노트
인쇄 미리보기

반응식

HRID 1713397 반응식
[C:1]1(=[O:11])[C:10]2[CH:5]([CH2:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][NH:2]1.[Br:12]Br.C([O-])(O)=O.[Na+]>C(Cl)(Cl)Cl>[Br:12][C:4]1[C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][C:10]=2[C:1](=[O:11])[NH:2][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24408BromineHCID 516892Sodium BicarbonateHCID 66591041HCID 66591041, 화합물2회

생성물 1

HCID 594638144-bromo-5,6,7,8-tetrahydro-1(2H)-Isoquinolinone수율 96.4%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

32.4 g (217 mmol) of tetrahydroisoquinolinone (compound 5) is dissolved in 300 ml of chloroform at 5° C. and then 11.2 ml (34.7 g, 217 mmol) of bromine, dissolved in 150 ml of chloroform, are added dropwise over the course of 1 h. The mixture is stirred while cooling in ice for a further hour and then neutralized with 150 ml of saturated NaHCO3 solution and filtered with suction. The organic phase of the filtrate is extracted with dichloromethane and concentrated. The residue is mixed with ethyl acetate, filtered off with suction and dried together with the first residue in a vacuum drying oven at 45° C. 47.7 g (96%) of colorless bromide are obtained.

후처리

  1. additionare added dropwise over the course of 1 h
  2. temperaturewhile cooling in ice for a further hour
  3. filtrationfiltered with suction
  4. extractionThe organic phase of the filtrate is extracted with dichloromethane
  5. concentrationconcentrated
  6. additionThe residue is mixed with ethyl acetate
  7. filtrationfiltered off with suction
  8. customdried together with the first residue in a vacuum
  9. customdrying oven at 45° C

출처 및 근거

ORD 기록
ord-3db7efe3e18e47fab619b84bcd5d9e40
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07795278B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트