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

Diethylaluminum chloride → HCID 21892018, 화합물

HRID 1007860
노트
인쇄 미리보기

반응식

HRID 1007860 반응식
[CH3:1][C:2]1[C:3](=[O:23])[N:4]2[C:16](=[CH:17][C:18]=1[C:19](=[O:22])[CH2:20][CH3:21])[C:7]1=[N:8][C:9]3[C:14]([CH:15]=[C:6]1[CH2:5]2)=[CH:13][CH:12]=[CH:11][CH:10]=3.Cl[Al](CC)CC.Br[CH2:31][C:32]([O:34][CH2:35][CH3:36])=[O:33].[K].C(C(C(C([O-])=O)O)O)([O-])=O.[Na+].[Na+]>O1CCCC1.[Zn].C([O-])(=O)C.[Ag+].C(O)C>[OH:22][C:19]([C:18]1[CH:17]=[C:16]2[N:4]([CH2:5][C:6]3[C:7]2=[N:8][C:9]2[C:14]([CH:15]=3)=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:3](=[O:23])[C:2]=1[CH3:1])([CH2:20][CH3:21])[CH2:31][C:32]([O:34][CH2:35][CH3:36])=[O:33]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 5

HCID 7277Diethylaluminum chlorideHCID 7748Ethyl bromoacetateHCID 13355Disodium 2,3-dihydroxybutanedioateHCID 1940068-Methyl-7-propanoylindolizino[1,2-b]quinolin-9(11H)-oneHCID 5462222Potassium

생성물 1

HCID 21892018HCID 21892018, 화합물수율 16.6%

시약·촉매·용매 4

HCID 11246Silver acetate촉매HCID 23994Zinc촉매HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

A suspension of zinc (1.25 g, 19.1 mmol); 8-methyl-7-propionylindolizino [1,2-b]quinoline-9-(11H)-one (500 mg, 1.43 mmol, as obtained by Kingsburry, W. D., Tetrahedron Lett. 29:6847 (1988)) and silver acetate (250 mg, 1.50 mmol) in anhydrous tetrahydrofuran (10 ml) is agitated at ambient temperature under an argon atmosphere. After 10 minutes, the reaction mixture is activated by the dropwise addition of a molar solution of chlorodiethylaluminium (10 ml, 10 mmol), then ethyl bromoacetate (1.25 ml, 11.3 mmol) is added dropwise and the resultant mixture is left to react for another 5 hours. The reaction is stopped by the successive addition of ethyl alcohol (10 ml) and a saturated solution of potassium and sodium tartrate (10 ml). The resultant mixture is agitated for another hour, filtered and concentrated under reduced pressure. The residue is taken up in dichloromethane (30 ml). washed with water, dried, concentrated and purified by column chromatography (SiO2, CH2Cl2/MeOH:98/2), which produces 93 mg (15%) of desired product in the form of a pale yellow solid, m.p. 185-188° C.

후처리

  1. customto react for another 5 hours
  2. filtrationfiltered
  3. concentrationconcentrated under reduced pressure
  4. washwashed with water
  5. customdried
  6. concentrationconcentrated
  7. custompurified by column chromatography (SiO2, CH2Cl2/MeOH:98/2), which

출처 및 근거

ORD 기록
ord-ca8e0b077abf42b28cabbb52aab56bb9
출처 데이터셋
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06797715B1

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트