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4-(4-Acetyl-1-piperazinyl)-2-(methyloxy)aniline → HCID 72546716、化合物

HRID 1496971
ノート
印刷プレビュー

反応式

HRID 1496971 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][N:11]([C:14](=[O:16])[CH3:15])[CH2:10][CH2:9]2)=[CH:4][C:3]=1[O:17][CH3:18].Cl[C:20]1[N:25]=[C:24]([NH:26][C:27]2[CH:32]=[CH:31][C:30]([N:33]3[CH2:38][CH2:37][N:36]([C:39](=[O:41])[CH3:40])[CH2:35][CH2:34]3)=[CH:29][C:28]=2[O:42][CH2:43][CH3:44])[C:23]([Cl:45])=[CH:22][N:21]=1>C(OC(O)C)C.Cl>[C:39]([N:36]1[CH2:35][CH2:34][N:33]([C:30]2[CH:31]=[CH:32][C:27]([NH:26][C:24]3[C:23]([Cl:45])=[CH:22][N:21]=[C:20]([NH:1][C:2]4[CH:7]=[CH:6][C:5]([N:8]5[CH2:13][CH2:12][N:11]([C:14](=[O:16])[CH3:15])[CH2:10][CH2:9]5)=[CH:4][C:3]=4[O:17][CH3:18])[N:25]=3)=[C:28]([O:42][CH2:43][CH3:44])[CH:29]=2)[CH2:38][CH2:37]1)(=[O:41])[CH3:40]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 552327374-(4-Acetyl-1-piperazinyl)-2-(methyloxy)anilineHCID 118105738HCID 118105738、化合物

生成物 1

HCID 72546716HCID 72546716、化合物

試薬・触媒・溶媒 1

HCID 19698338HCID 19698338、化合物溶媒

実験手順

1-(4-(4-amino-3-methoxyphenyl)piperazin-1-yl)ethanone (40 mg) prepared in Preparation Example 1 and 1-(4-(4-(2,5-dichloropyrimidine-4-ylamino)-3-ethoxyphenyl)piperazin-1-yl)ethanone (50 mg) prepared in Preparation Example 15 were dissolved in 0.08M HCl ethoxyethanol solution (1.2 mL), and allowed to react at 115° C. overnight. Upon completion of the reaction, the solvent of the mixture was removed under reduced pressure, diluted with ethyl acetate, neutralized with an aqueous saturated sodium carbonate solution, water was removed from the organic layer with sodium sulfate, and the solvent was removed under reduced pressure. The mixture was purified by column chromatography to obtain a target compound.

後処理

  1. customprepared in Preparation Example 15
  2. customto react at 115° C. overnight
  3. customUpon completion of the reaction
  4. customthe solvent of the mixture was removed under reduced pressure
  5. additiondiluted with ethyl acetate
  6. customwas removed from the organic layer with sodium sulfate
  7. customthe solvent was removed under reduced pressure
  8. customThe mixture was purified by column chromatography
  9. customto obtain a target compound

出典と根拠

ORDレコード
ord-38dfc35b5e5d4bbeacce2517d28a0079
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09199944B2

反応ノート

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