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Sodium Chloride → 6-(4-Benzyl-1-piperazinylcarbonyl)-3,4-dihydrocarbostyril

HRID 358498
ノート
印刷プレビュー

反応式

HRID 358498 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.ClC(OCC(C)C)=O.[CH2:23]([N:30]1[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.[Cl-].[Na+]>CN(C)C=O.C(OCC)C.C(N(CC)CC)C>[CH2:23]([N:30]1[CH2:35][CH2:34][N:33]([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])[CH2:32][CH2:31]1)[C:24]1[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 5234Sodium ChlorideHCID 62365Isobutyl chloroformateHCID 759941-BenzylpiperazineHCID 71319092-Oxo-1,2,3,4-tetrahydroquinoline-6-carboxylic acid

生成物 1

HCID 131953356-(4-Benzyl-1-piperazinylcarbonyl)-3,4-dihydrocarbostyril収率 37.2%

試薬・触媒・溶媒 3

HCID 3283
Diethyl Ether
溶媒
HCID 6228Dimethylformamide溶媒3 回
HCID 8471Triethylamine溶媒

実験手順

To a solution of 50 ml of dimethylformamide with 5.0 g of 6-carboxy-3,4-dihydrocarbostyril and 4 ml of triethylamine, 3.87 g of isobutyl chloroformate in 2 ml of dimethylformamide solution was added dropwise. After stirring at a room temperature for 30 minutes, 5.5 g of benzylpiperazine in 3 ml of dimethylformamide solution was added to the former solution and stirred at a room temperature for 30 minutes, then stirred continuously at 50°-60° C. for 1 hour. The reaction mixture was poured into a voluminous amount of a saturated sodium chloride aqueous solution and extracted with chloroform and the chloroform extract was washed with water and dried. After removal of the solvent, to the residue thus obtained was added diethyl ether to crystallize the residue and recrystallized from ethanol to obtain 3.4 g of 6-(4-benzyl-1-piperazinylcarbonyl)-3,4-dihydrocarbostyril. Colorless needle-like crystals. Melting point: 198°-200° C.

後処理

  1. stirringstirred at a room temperature for 30 minutes
  2. stirringstirred continuously at 50°-60° C. for 1 hour
  3. extractionextracted with chloroform
  4. extractionthe chloroform extract
  5. washwas washed with water
  6. customdried
  7. customAfter removal of the solvent
  8. customto the residue thus obtained
  9. customto crystallize the residue
  10. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-2ffd4ec607d641519f3b7bf60999cdc7
出典データセット
uspto-grants-1984_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04468402

反応ノート

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