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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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Water → HCID 54547942、化合物

HRID 582320
ノート
印刷プレビュー

反応式

HRID 582320 の反応式
CO[C:3](=[O:28])[C:4]1[CH:9]=[CH:8][C:7]([C:10]([N:12]2[CH2:17][CH2:16][N:15]([C:18]3[C:23]([NH:24][CH:25]([CH3:27])[CH3:26])=[CH:22][CH:21]=[CH:20][N:19]=3)[CH2:14][CH2:13]2)=[O:11])=[CH:6][CH:5]=1.[NH2:29][CH2:30][CH2:31][N:32]1[CH2:37][CH2:36][O:35][CH2:34][CH2:33]1.O>C(O)C.C(#N)C>[CH:25]([NH:24][C:23]1[C:18]([N:15]2[CH2:16][CH2:17][N:12]([C:10]([C:7]3[CH:8]=[CH:9][C:4]([C:3](=[O:28])[NH:29][CH2:30][CH2:31][N:32]4[CH2:37][CH2:36][O:35][CH2:34][CH2:33]4)=[CH:5][CH:6]=3)=[O:11])[CH2:13][CH2:14]2)=[N:19][CH:20]=[CH:21][CH:22]=1)([CH3:27])[CH3:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 962WaterHCID 4082852-MorpholinoethylamineHCID 537116704-[1-[3-(Isopropylamino)-2-pyridyl]piperazin-4-yl-carbonyl]benzoic acid methyl ester

生成物 1

HCID 54547942HCID 54547942、化合物収率 81%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 6342
Acetonitrile
溶媒

実験手順

4-[1-[3-(Isopropylamino)-2-pyridyl]piperazin-4-yl-carbonyl]benzoic acid methyl ester (1.2 g) was dissolved in a co-solvent of ethanol (10 ml) and acetonitrile (20 ml), and 4-(2-aminoethyl)morpholine (0.82 g) was added. The reaction mixture was heated to reflux for 15 hours and cooled. After excess of water was added to the solution at 30° C. to precipitate the crystals, the solution was stirred for 1 hour. Then, the solution was again cooled slowly, stirred at 10~15° C. for 2 hours and filtered. The filtered crystal was washed with preheated water(40° C.) and was recrystallized using isopropanol and ether, filtered and dried to give 1.22 g (yield: 81%) of the desired compound.

後処理

  1. additionwas added
  2. temperatureThe reaction mixture was heated
  3. temperatureto reflux for 15 hours
  4. temperaturecooled
  5. customto precipitate the crystals
  6. temperatureThen, the solution was again cooled slowly
  7. stirringstirred at 10~15° C. for 2 hours
  8. filtrationfiltered
  9. washThe filtered crystal was washed with preheated water(40° C.)
  10. customwas recrystallized
  11. filtrationfiltered
  12. customdried

出典と根拠

ORDレコード
ord-d9ba63fa0b444ce299a0bfb70e6c7b93
出典データセット
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05922871

反応ノート

読み込み中…

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