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Cyclohexanecarbonyl chloride → HCID 21326339, 화합물

HRID 26032
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HRID 26032 반응식
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([OH:13])=[C:6]2[C:11]=1[NH:10][C:9](=[O:12])[CH2:8][CH2:7]2.[CH:14]1([C:20](Cl)=[O:21])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1>N1C=CC=CC=1>[CH:14]1([C:20]([NH:1][C:2]2[CH:3]=[CH:4][C:5]([OH:13])=[C:6]3[C:11]=2[NH:10][C:9](=[O:12])[CH2:8][CH2:7]3)=[O:21])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1
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참가 물질

4

반응물 2

HCID 75938Cyclohexanecarbonyl chlorideHCID 213263108-Amino-5-hydroxy-3,4-dihydrocarbostyril

생성물 1

HCID 21326339HCID 21326339, 화합물수율 38.1%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

10.7 g of 8-amino-5-hydroxy-3,4-dihydrocarbostyril was dissolved in 100 ml of pyridine, and 10.0 g of cyclohexylcarbonyl chloride was added to the solution while vigorously stirring at room temperature followed by stirring at 50° C. for 30 minutes. The precipitated crystals were recovered by filtration, washed with ethanol, dried and dissolved in 200 ml of a 10% aqueous sodium hydroxide solution. Activated carbon was added to the solution, and the mixture was stirred and filtered. The filtrate was rendered acidic with hydrochloric acid under ice cooling, and the precipitated crystals were recovered by filtration, washed with water and dried. Recrystallization from methanol yielded 6.6 g of 8-cyclohexylcarbonylamino-5-hydroxy-3,4-dihydrocarbostyril as colorless amorphous crystals having a melting point of 304.2°-304.8° C.

후처리

  1. stirringby stirring at 50° C. for 30 minutes
  2. filtrationThe precipitated crystals were recovered by filtration
  3. washwashed with ethanol
  4. customdried
  5. dissolutiondissolved in 200 ml of a 10% aqueous sodium hydroxide solution
  6. additionActivated carbon was added to the solution
  7. stirringthe mixture was stirred
  8. filtrationfiltered
  9. filtrationthe precipitated crystals were recovered by filtration
  10. washwashed with water
  11. customdried
  12. customRecrystallization from methanol

출처 및 근거

ORD 기록
ord-ed3e672efcb94cddae4823c564ec1843
출처 데이터셋
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04147869

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