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

Thionyl Chloride → HCID 13295785, 화합물

HRID 1193663
노트
인쇄 미리보기

반응식

HRID 1193663 반응식
[N:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][C:9]=2[O:11][CH2:12][CH2:13][CH2:14]O)[CH:4]=[CH:3][CH:2]=1.S(Cl)([Cl:18])=O>C1C=CC=CC=1>[Cl:18][CH2:14][CH2:13][CH2:12][O:11][C:9]1[CH:8]=[CH:7][CH:6]=[C:5]2[C:10]=1[N:1]=[CH:2][CH:3]=[CH:4]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 132957843-(8-Quinolinyloxy)-1-propanol

생성물 1

HCID 13295785HCID 13295785, 화합물

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A solution of 3-(8-quinolinyloxy)-1-propanol (32.0 g, 0.158 mole) and thionyl chloride (24.0 g, 0.203 mole) was heated at reflux for 5 hours in 300 ml of dry benzene (dried over 4 A molecular sieves). The reaction mixture was cooled to room temperature and then stripped to dryness. The residue was treated with potassium carbonate solution (30 g in 500 ml of water). The gummy residue was dissolved in chloroform and extracted with the potassium carbonate solution. The chloroform layer was dried over anhydrous sodium sulfate, filtered, and solvent removed to give a dark mass which crystallized. The mass was treated with 500 ml of boiling hexane. The hexane layer was decanted off from insoluble oil. A white solid crystallized on cooling, the hexane layer was filtered off. The solid was dried in vacuo at room temperature overnight to give 26.69 g (76.2%) of white cyrstalline solid, m.p. 69°-71° C.

후처리

  1. customdried over 4 A molecular sieves)
  2. additionThe residue was treated with potassium carbonate solution (30 g in 500 ml of water)
  3. dissolutionThe gummy residue was dissolved in chloroform
  4. extractionextracted with the potassium carbonate solution
  5. dry with materialThe chloroform layer was dried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. customsolvent removed
  8. customto give a dark mass which
  9. customcrystallized
  10. additionThe mass was treated with 500 ml of boiling hexane
  11. customThe hexane layer was decanted off from insoluble oil
  12. customA white solid crystallized
  13. temperatureon cooling
  14. filtrationthe hexane layer was filtered off
  15. customThe solid was dried in vacuo at room temperature overnight
  16. customto give 26.69 g (76.2%) of white cyrstalline solid, m.p. 69°-71° C.

출처 및 근거

ORD 기록
ord-41fa86e6475645fa8b1e1f11c948bfec
출처 데이터셋
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04810713

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트