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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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1,4-Dioxane → HCID 20339592、化合物

HRID 1395547
ノート
印刷プレビュー

反応式

HRID 1395547 の反応式
C([Li])CCC.O1CCOCC1.[CH3:12][N:13]([CH3:24])[C:14]([NH:16][C:17]1[CH:22]=[CH:21][CH:20]=[C:19]([NH2:23])[N:18]=1)=[O:15].Cl.[CH:26]([N:29]([CH:33]([CH3:35])[CH3:34])[CH2:30][CH2:31]Cl)([CH3:28])[CH3:27]>CCCCCC.C(O)C>[CH3:12][N:13]([CH3:24])[C:14]([N:16]([CH2:31][CH2:30][N:29]([CH:33]([CH3:35])[CH3:34])[CH:26]([CH3:28])[CH3:27])[C:17]1[CH:22]=[CH:21][CH:20]=[C:19]([NH2:23])[N:18]=1)=[O:15]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 312751,4-DioxaneHCID 779422-Chloroethyldiisopropylammonium chlorideHCID 20339614N'-(6-Aminopyridin-2-yl)-N,N-dimethylureaHCID 178418339Butyllithium2 回

生成物 1

HCID 20339592HCID 20339592、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒
HCID 8058
Hexane
溶媒

反応条件

温度
-25 °C

実験手順

Under a nitrogen atmosphere, n-butyl lithium solution (15.5 ml., 0.025 mole) is added dropwise with stirring to a dioxane (50 ml.) solution of N,N-dimethyl-N'-(6-amino-2-pyridyl)urea (4.5 g., 0.025 mole) at 10° C. Then 2-diisopropylaminoethyl chloride hydrochloride (55.5 g., 0.275 mole) is added followed by another portion of n-butyl lithium (15.5 ml., 0.025 mole). The mixture is heated at reflux over night. Ethanol (30 ml.) is added with cooling and the mixture is filtered and concentrated in vacuo. The residue is treated with ether and is filtered to remove salts. Removal of the ether in vacuo gives 5.1 g. of viscous oil. The crude oil is taken up in hexane, filtered and cooled to -25° C. Filtration gives 1.5 g. of white solid, m.p. 86°-88° C.

後処理

  1. temperatureThe mixture is heated
  2. temperatureat reflux over night
  3. temperaturewith cooling
  4. filtrationthe mixture is filtered
  5. concentrationconcentrated in vacuo
  6. additionThe residue is treated with ether
  7. filtrationis filtered
  8. customto remove salts
  9. customRemoval of the ether in vacuo
  10. customgives 5.1 g
  11. filtrationfiltered
  12. filtrationFiltration
  13. customgives 1.5 g

出典と根拠

ORDレコード
ord-a3ac5a4c45e9474296969eb4ceb613ae
出典データセット
uspto-grants-1980_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04203988

反応ノート

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