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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
ノート
印刷プレビュー

反応式

HRID 4174 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 62652Cuprous chloride触媒
HCID 31275
1,4-Dioxane
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-301ed65de99248bebe2bd6e6ac674570
出典データセット
uspto-grants-1988_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04724236

反応ノート

読み込み中…

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