Sodium Hydroxide → HCID 22643234、化合物

HRID 2414755ノート

反応式

HRID 2414755 の反応式
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([NH:12]C(=O)C)[CH:10]=2)[N:5]=[C:4]([C:16]2[CH:21]=[CH:20][C:19]([CH:22]3[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]3)=[CH:18][CH:17]=2)[CH:3]=1.[OH-].[Na+]>Cl>[CH:22]1([C:19]2[CH:18]=[CH:17][C:16]([C:4]3[CH:3]=[C:2]([NH2:1])[C:11]4[C:6](=[CH:7][CH:8]=[C:9]([NH2:12])[CH:10]=4)[N:5]=3)=[CH:21][CH:20]=2)[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27]1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 22643183HCID 22643183、化合物

生成物 1

HCID 22643234HCID 22643234、化合物収率 87.5%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

反応条件

温度
95 °C

実験手順

N-[4-Amino-2-(4-cyclohexylphenyl)-quinolin-6-yl]-acetamide (22 g) was placed in a 1 L flask to which 500 mL of 6 N HCl was added and the mixture heated with stirring to 95° C. for 18 hrs. After this time, the solution was cooled in ice and was then cautiously neutralized with concentrated NaOH solution, followed by adjustment to pH 9.5. The solution was then poured into a 2 L separatory funnel and extracted with ethyl acetate. The organic layer was then dried over Na2SO4, filtered and concentrated to give 17 g of the desired product. Repeated crystallization using methanol, methylene chloride and hexane provided 9.0 g (41%) of the pure title compound.

後処理

  1. additionwas added
  2. temperaturethe mixture heated
  3. temperatureAfter this time, the solution was cooled in ice
  4. additionThe solution was then poured into a 2 L separatory funnel
  5. extractionextracted with ethyl acetate
  6. dry with materialThe organic layer was then dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-46a1bce4257349b38391b9a69d214e9d
出典データセット
uspto-grants-2004_11
特許番号
US06815447B2

反応ノート

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