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Hydrochloric Acid → 6-(4-Geranyl-1-piperazinylcarbonyl)-3,4-dihydrocarbostyril hydrochloride

HRID 231105
ノート
印刷プレビュー

反応式

HRID 231105 の反応式
[C:1]([C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[NH:10][C:9](=[O:14])[CH2:8][CH2:7]2)([OH:3])=O.C1(N=C=NC2CCCCC2)CCCCC1.[CH2:30]([N:40]1[CH2:45][CH2:44][NH:43][CH2:42][CH2:41]1)/[CH:31]=[C:32](/[CH2:34][CH2:35][CH:36]=[C:37]([CH3:39])[CH3:38])\[CH3:33].[ClH:46]>O1CCOCC1.C(O)C.C(Cl)(Cl)Cl.C(OCC)C>[ClH:46].[CH2:30]([N:40]1[CH2:41][CH2:42][N:43]([C:1]([C:4]2[CH:5]=[C:6]3[C:11](=[CH:12][CH:13]=2)[NH:10][C:9](=[O:14])[CH2:8][CH2:7]3)=[O:3])[CH2:44][CH2:45]1)/[CH:31]=[C:32](/[CH2:34][CH2:35][CH:36]=[C:37]([CH3:38])[CH3:39])\[CH3:33]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 313Hydrochloric Acid2 回HCID 10868DicyclohexylcarbodiimideHCID 71319092-Oxo-1,2,3,4-tetrahydroquinoline-6-carboxylic acidHCID 14497703Geranylpiperazine

生成物 1

HCID 200345276-(4-Geranyl-1-piperazinylcarbonyl)-3,4-dihydrocarbostyril hydrochloride

試薬・触媒・溶媒 4

HCID 702
Ethanol
溶媒
HCID 3283Diethyl Ether溶媒
HCID 6212Chloroform溶媒
HCID 312751,4-Dioxane溶媒

実験手順

1.0 Gram of 6-carboxy-3,4-dihydrocarbostyril, 1.3 g of DCC (dicyclohexylcarbodiimide) and 1.4 g of geranylpiperazine were suspended in 10 ml of dioxane, and the suspension was stirred at 60°-70° C. for 5 hours. After the reaction was finished, the solvent was removed from the reaction mixture by evaporation, then to the residue thus obtained was added a certain amount of diethyl ether and the crystals formed were removed by filtration. The mother liquor was concentrated, and the residue thus obtained was dissolved by adding chloroform, the chloroform solution was washed with water and an aqueous solution saturated with sodium chloride. The chloroform solution was dried with anhydrous sodium sulfate, then the solvent was removed by evaporation. To the residue thus obtained was added 20 ml of ethanol, and converted into hydrochloride with 1.3 ml of concentrated hydrochloric acid. Recrystallized from ethanol-water to obtain 340 mg of 6-(4-geranyl-1-piperazinylcarbonyl)-3,4-dihydrocarbostyril.hydrochloride. monohydrate. Colorless needle-like crystals. Melting point: 265°-266° C. (dec.).

後処理

  1. customthe solvent was removed from the reaction mixture by evaporation
  2. customto the residue thus obtained
  3. customthe crystals formed
  4. customwere removed by filtration
  5. concentrationThe mother liquor was concentrated
  6. customthe residue thus obtained
  7. dissolutionwas dissolved
  8. washthe chloroform solution was washed with water
  9. dry with materialThe chloroform solution was dried with anhydrous sodium sulfate
  10. customthe solvent was removed by evaporation
  11. customTo the residue thus obtained
  12. customRecrystallized from ethanol-water

出典と根拠

ORDレコード
ord-3cdefc7e369a4713b6b9a2bf2df4c8bd
出典データセット
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04845100

反応ノート

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