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Triethylamine → HCID 21075825、化合物

HRID 1373956
ノート
印刷プレビュー

反応式

HRID 1373956 の反応式
[C:1]([O:5][C:6]([CH3:9])([CH3:8])[CH3:7])(=[O:4])[NH:2][NH2:3].C(N(CC)CC)C.[CH2:17]([O:24][C:25]1[CH:34]=[C:33]2[C:28]([C:29](Cl)=[C:30]([N+:35]([O-:37])=[O:36])[CH:31]=[N:32]2)=[CH:27][CH:26]=1)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>ClCCl.O.C(Cl)(Cl)Cl>[CH2:17]([O:24][C:25]1[CH:34]=[C:33]2[C:28]([C:29]([NH:3][NH:2][C:1]([O:5][C:6]([CH3:9])([CH3:8])[CH3:7])=[O:4])=[C:30]([N+:35]([O-:37])=[O:36])[CH:31]=[N:32]2)=[CH:27][CH:26]=1)[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 8471TriethylamineHCID 70091tert-Butyl carbazateHCID 210757517-(Benzyloxy)-4-chloro-3-nitroquinoline

生成物 1

HCID 21075825HCID 21075825、化合物収率 57.2%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6212Chloroform溶媒
HCID 6344
Dichloromethane
溶媒
2 回

実験手順

A solution of tert-butyl carbazate (33.1 g, 251 mmol) in 150 mL of dichloromethane was treated with triethylamine (66.5 mL, 502 mmol). The solution was placed under an atmosphere of nitrogen and cooled in a cold-water bath. The solution was treated with a solution of 7-benzyloxy-4-chloro-3-nitroquinoline (71.7 g, 228 mmol) in 350 mL of dichloromethane over 1 h. The reaction was stirred and allowed to warm to ambient temperature. After 15 h, the reaction was diluted with 200 mL of water and 250 mL of CHCl3 and the phases were separated. The organic portion was washed with water (200 mL), brine (200 mL), dried over Na2SO4, filtered and concentrated under reduced pressure to yield an orange solid. The solid was recrystallized from dichloromethane to yield 53.5 g of tert-butyl N′-(7-benzyloxy-3-nitroquinolin-4-yl)hydrazinecarboxylate as yellow crystals.

後処理

  1. temperaturecooled in a cold-water bath
  2. customthe phases were separated
  3. washThe organic portion was washed with water (200 mL), brine (200 mL)
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customto yield an orange solid
  8. customThe solid was recrystallized from dichloromethane

出典と根拠

ORDレコード
ord-25088d4f06614f8e8d9c13425dbfe9c2
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07163947B2

反応ノート

読み込み中…

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