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Hydrochloric Acid → 6-(3-Aminopropoxy)carbostyril

HRID 1856744
ノート
印刷プレビュー

反応式

HRID 1856744 の反応式
C1(=O)[N:5]([CH2:6][CH2:7][CH2:8][O:9][C:10]2[CH:11]=[C:12]3[C:17](=[CH:18][CH:19]=2)[NH:16][C:15](=[O:20])[CH:14]=[CH:13]3)C(=O)C2=CC=CC=C12.O.NN.Cl>C(O)C>[NH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:11]=[C:12]2[C:17](=[CH:18][CH:19]=1)[NH:16][C:15](=[O:20])[CH:14]=[CH:13]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 24654Hydrazine hydrate (1:1)HCID 117724126-(3-Phthalimidopropoxy)carbostyril

生成物 1

HCID 100136326-(3-Aminopropoxy)carbostyril収率 74.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a suspension of 6-(3-phthalimidopropoxy)carbostyril (300 g) in ethanol (3 liters) is added hydrazine monohydrate (46 g), and the mixture is refluxed for 8 hours. After the mixture is allowed to cool, the precipitated crystals are collected by filtration, suspended in water, and the suspension thus obtained is acidified with conc. hydrochloric acid, and stirred for one hour. The insoluble materials are removed by filtration, and the filtrate is concentrated under reduced pressure to remove the solvent. The residue is neutralized to pH 7 with a 15% aqueous sodium hydroxide solution. The precipitated crystals are collected by filtration, and washed successively with ethanol and diethyl ether, and dried to give 6-(3-aminopropoxy)carbostyril (140 g) as a white powder.

後処理

  1. temperaturethe mixture is refluxed for 8 hours
  2. temperatureto cool
  3. filtrationthe precipitated crystals are collected by filtration
  4. customthe suspension thus obtained
  5. customThe insoluble materials are removed by filtration
  6. concentrationthe filtrate is concentrated under reduced pressure
  7. customto remove the solvent
  8. filtrationThe precipitated crystals are collected by filtration
  9. washwashed successively with ethanol and diethyl ether
  10. customdried

出典と根拠

ORDレコード
ord-e6fddc6f72094a0381cd978cdd7b4772
出典データセット
uspto-grants-2000_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06143763

反応ノート

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