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Sodium Chloride → HCID 22989248、化合物

HRID 1169043
ノート
印刷プレビュー

反応式

HRID 1169043 の反応式
[C:1]1([CH:7]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][OH:17])[CH2:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H-].[Na+].Cl[C:27]1[CH:28]=[CH:29][C:30]2[N:31]([CH:33]=[C:34]([O:36][CH3:37])[N:35]=2)[N:32]=1.[Cl-].[Na+]>CN(C)C=O>[C:18]1([CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[N:8]2[CH2:9][CH2:10][N:11]([CH2:14][CH2:15][CH2:16][O:17][C:27]3[CH:28]=[CH:29][C:30]4[N:31]([CH:33]=[C:34]([O:36][CH3:37])[N:35]=4)[N:32]=3)[CH2:12][CH2:13]2)[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1
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

6

反応物 4

HCID 5234Sodium ChlorideHCID 24758Sodium hydrideHCID 155241464-Benzhydryl-1-piperazinepropanolHCID 229893386-Chloro-2-methoxyimidazo[1,2-b]pyridazine

生成物 1

HCID 22989248HCID 22989248、化合物収率 26.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒

反応条件

温度
60 °C

実験手順

251 mg of 4-(diphenylmethyl)-1-piperazinepropanol was dissolved in 14 ml of N,N-dimethylformamide; 36 mg of a 60% sodium hydride dispersion in mineral oil was added, followed by stirring at 60° C. for 30 minutes. After cooling, 149 mg of 6-chloro-2-methoxyimidazo[1,2-b]pyridazine was added, followed by stirring at 90° C. for 4.5 hours. After cooling, ice water and sodium chloride were added, followed by extraction with ethyl acetate-tetrahydrofuran (1:2); the extract was washed with saturated saline, dried over magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography and eluted with ethyl acetate. The desired fraction was collected; the crystal precipitated was recrystallized from ethyl acetate to yield 99 mg of the title compound.

後処理

  1. temperatureAfter cooling
  2. stirringby stirring at 90° C. for 4.5 hours
  3. temperatureAfter cooling
  4. extractionfollowed by extraction with ethyl acetate-tetrahydrofuran (1:2)
  5. washthe extract was washed with saturated saline
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. washeluted with ethyl acetate
  9. customThe desired fraction was collected
  10. customthe crystal precipitated
  11. customwas recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-b272c3576dc4491bb3a6884ead0d789f
出典データセット
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06627630B1

反応ノート

読み込み中…

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