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Formaldehyde → HCID 21270045、化合物

HRID 1194347
ノート
印刷プレビュー

反応式

HRID 1194347 の反応式
[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([C:11](=[O:13])[CH3:12])=[C:3]1[CH3:14].[CH2:15]=O.Cl.[CH3:18][NH:19][CH3:20]>C(O)C>[CH3:18][N:19]([CH3:15])[CH2:20][CH2:12][C:11]([C:4]1[C:5]2[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=2)[N:2]([CH3:1])[C:3]=1[CH3:14])=[O:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 712FormaldehydeHCID 10473Dimethylamine, hydrochlorideHCID 2857551-(1,2-dimethyl-1H-indol-3-yl)ethanone

生成物 1

HCID 21270045HCID 21270045、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 1-(1,2-dimethyl-1H-indol-3-yl)-1-ethanone (0.9 g), paraformaldehyde (0.43 g) and dimethylamine hydrochloride (1.2 g) in ethanol (60 ml) was heated at reflux for 18 h, cooled, and the solvent evaporated in vacuo. The residue was partitioned between sodium carbonate (2N; 50 ml) and ethyl acetate (2×50 ml) and the combined organic extracts were dried and evaporated in vacuo to give an oil. This oil was chromatographed eluting with System A to give the title compound, which on standing gave crystals (0.9 g), m.p. 96°-98°.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 18 h
  3. temperaturecooled
  4. customthe solvent evaporated in vacuo
  5. customThe residue was partitioned between sodium carbonate (2N; 50 ml) and ethyl acetate (2×50 ml)
  6. customthe combined organic extracts were dried
  7. customevaporated in vacuo
  8. customto give an oil
  9. customThis oil was chromatographed
  10. washeluting with System A

出典と根拠

ORDレコード
ord-e02d5304419841458093e9e28ad2f016
出典データセット
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04814344

反応ノート

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