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Isobutyl chloroformate → 6-[3-(4-Cyclohexyl-1-piperazylcarbonyl)propoxy]carbostyril

HRID 1903192
ノート
印刷プレビュー

反応式

HRID 1903192 の反応式
[C:1]([CH2:4][CH2:5][CH2:6][O:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][CH:17]=1)[NH:14][C:13](=[O:18])[CH:12]=[CH:11]2)([OH:3])=O.C1CCN2C(=NCCC2)CC1.ClC(OCC(C)C)=O.[CH:38]1([N:44]2[CH2:49][CH2:48][NH:47][CH2:46][CH2:45]2)[CH2:43][CH2:42][CH2:41][CH2:40][CH2:39]1>CO.C(Cl)(Cl)Cl>[CH:38]1([N:44]2[CH2:49][CH2:48][N:47]([C:1]([CH2:4][CH2:5][CH2:6][O:7][C:8]3[CH:9]=[C:10]4[C:15](=[CH:16][CH:17]=3)[NH:14][C:13](=[O:18])[CH:12]=[CH:11]4)=[O:3])[CH2:46][CH2:45]2)[CH2:43][CH2:42][CH2:41][CH2:40][CH2:39]1
参加物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 62365Isobutyl chloroformateHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 872981-CyclohexylpiperazineHCID 128663424-((2-Oxo-1,2-dihydroquinolin-6-yl)oxy)butanoic acid

生成物 1

HCID 131079796-[3-(4-Cyclohexyl-1-piperazylcarbonyl)propoxy]carbostyril収率 49.8%

試薬・触媒・溶媒 2

HCID 887
Methanol
溶媒
HCID 6212Chloroform溶媒2 回

実験手順

Into 200 ml of chloroform were added 5 g of 6-(3-carboxypropoxy)carbostyril and 3.2 g DBU. The outside of the reaction vessel containing the above mentioned mixture was ice-cooled and 2.8 g of isobutyl chloroformate was added dropwise to the mixture under stirring condition. After the addition operation, the reaction mixture was further stirred for 1 hour, then 3.7 g of N-cyclohexylpiperazine was added dropwise at a room temperature, and the reaction was continued for 5 hours. After the reaction was completed, the reaction mixture was washed with 1% NaOH aqueous solution and water, then dried with anhydrous sodium sulfate. The drying agent was removed by filtration and the mother liquor was concentrated. The residue thus obtained was treated by a silica-gel column chromatography (solvent used was a mixture of chloroform:methanol=30:1) to obtain elute. The elute was concentrated and the residue was recrystallized from water-containing methanol to obtain 4 g of 6-[3-(4-cyclohexyl-1-piperazylcarbonyl)propoxy]carbostyril in the form of colorless needle-like crystals. Melting point: 184.5°-186° C.

後処理

  1. additionThe outside of the reaction vessel containing the
  2. temperaturecooled
  3. stirringAfter the addition operation, the reaction mixture was further stirred for 1 hour
  4. washthe reaction mixture was washed with 1% NaOH aqueous solution and water
  5. dry with materialdried with anhydrous sodium sulfate
  6. customThe drying agent was removed by filtration
  7. concentrationthe mother liquor was concentrated
  8. customThe residue thus obtained
  9. additionwas treated by a silica-gel column chromatography (solvent
  10. washelute
  11. concentrationThe elute was concentrated
  12. customthe residue was recrystallized from water-
  13. additioncontaining methanol

出典と根拠

ORDレコード
ord-12658c25651341c39330c14c47f6784a
出典データセット
uspto-grants-1984_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04435404

反応ノート

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