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Formaldehyde → 5,11-Dihydro-11-[1-oxo-6-(1-piperidinyl)-4-hexynyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one

HRID 4174
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인쇄 미리보기

반응식

HRID 4174 반응식
[O:1]=[C:2]([N:7]1[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=2[C:11](=[O:18])[NH:10][C:9]2[CH:19]=[CH:20][CH:21]=[N:22][C:8]1=2)[CH2:3][CH2:4][C:5]#[CH:6].[CH2:23]=O.[NH:25]1[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]1>[Cu]Cl.O1CCOCC1>[O:1]=[C:2]([N:7]1[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=2[C:11](=[O:18])[NH:10][C:9]2[CH:19]=[CH:20][CH:21]=[N:22][C:8]1=2)[CH2:3][CH2:4][C:5]#[C:6][CH2:23][N:25]1[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 712FormaldehydeHCID 8082PiperidineHCID 137291885,11-dihydro-11-[1-oxo-4-pentynyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one

생성물 1

HCID 137291895,11-Dihydro-11-[1-oxo-6-(1-piperidinyl)-4-hexynyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one

시약·촉매·용매 2

HCID 62652Cuprous chloride촉매
HCID 31275
1,4-Dioxane
용매

실험 절차

A mixture consisting of 9.6 g (0.03 mol) of 5,11-dihydro-11-[1-oxo-4-pentynyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one, 1.08 g (0.036 mol) of paraformaldehyde, 3.06 g (0.036 mol) of piperidine, 0.2 g of copper(I) chloride and 150 ml of dioxan is refluxed for 1 hour. After the reaction has ended the insoluble constituents are filtered off and the filtrate is evaporated to dryness in vacuo. The crude product is purified by column chromatography on silica gel (mobile phase: ethyl acetate, ethyl acetate+10% methanol). After recrystallisation from ethyl acetate, 2.7 g (21% of theory) of the desired compound are obtained, m.p. 197° C.

후처리

  1. temperatureis refluxed for 1 hour
  2. filtrationare filtered off
  3. customthe filtrate is evaporated to dryness in vacuo
  4. customThe crude product is purified by column chromatography on silica gel (mobile phase: ethyl acetate, ethyl acetate+10% methanol)
  5. customAfter recrystallisation from ethyl acetate, 2.7 g (21% of theory) of the desired compound
  6. customare obtained

출처 및 근거

ORD 기록
ord-301ed65de99248bebe2bd6e6ac674570
출처 데이터셋
uspto-grants-1988_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04724236

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