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Hydrochloric Acid → 8-Amino-5-morpholinoquinoline

HRID 2107311
ノート
印刷プレビュー

反応式

HRID 2107311 の反応式
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:16]=[CH:15][C:14]([N+:17]([O-])=O)=[C:13]3[C:8]=2[CH:9]=[CH:10][CH:11]=[N:12]3)[CH2:3][CH2:2]1.Cl.C(=O)([O-])[O-].[K+].[K+]>O>[NH2:17][C:14]1[CH:15]=[CH:16][C:7]([N:4]2[CH2:5][CH2:6][O:1][CH2:2][CH2:3]2)=[C:8]2[C:13]=1[N:12]=[CH:11][CH:10]=[CH:9]2
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 31356775-Morpholin-4-yl-8-nitro-quinoline

生成物 1

HCID 145011628-Amino-5-morpholinoquinoline収率 53%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

5-Morpholino-8-nitroquinoline, 3.90 g, was dissolved into 30 ml of water and 30 ml of hydrochloric acid. To this mixture 10.2 g of stannous chloride.dihydrate was added and the mixture was heated on a water bath under stirring for 1 hour. After cooling, the mixture was neutralized with potassium carbonate and extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate. Ethyl acetate was evaporated to produce 1.83 g (yield: 53%) of 8-amino-5-morpholinoquinoline. This compound was dissolved into 10 ml of water and 6 ml of concentrated HCl, and to the solution an aqueous solution containing 0.62 g of sodium nitrite was added dropwise while stirring at -15° C. The diazonium salt thus obtained was neutralized with sodium bicarbonate, and resulting product was added at 0° C. into an aqueous solution of cuprous cyanide (prepared from 2.0 g of cuprous chloride and 3.4 g of potassium cyanide). The mixture was stirred at the same temperature for 1 hour, then at 70° C. for 30 minutes to complete the reaction. The reaction mixture was extracted with ethyl acetate and the extract was dried over anhydrous sodium sulfate. Ethyl acetate was evaporated and the residue was refined by column chromatography on silica gel using a chloroform-n-hexane (3:2) mixed solvent as an eluent. The crystals thus obtained were recrystallized from ethanol to yield 0.12 g (yield: 6.2%) of 5-morpholino-8-quinolinecarbonitrile (Compound No. 13)

後処理

  1. temperaturethe mixture was heated on a water bath
  2. temperatureAfter cooling
  3. extractionextracted with ethyl acetate
  4. dry with materialThe extract was dried over anhydrous sodium sulfate
  5. customEthyl acetate was evaporated

出典と根拠

ORDレコード
ord-7c1c6ee1be78429f991bc8f5618fa9db
出典データセット
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04933447

反応ノート

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