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Hydrochloric Acid → 1-Ethyl-6,8-difluoro-1,4-dihydro-4-oxo-7-[3-(4-aminobenzenesulfonamido)-1-pyrrolidinyl]-3-quinolinecarboxylic acid

HRID 1290735
ノート
印刷プレビュー

反応式

HRID 1290735 の反応式
[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:33])=[C:10]([N:14]3[CH2:18][CH2:17][CH:16]([NH:19][S:20]([C:23]4[CH:28]=[CH:27][C:26]([NH:29]C(=O)C)=[CH:25][CH:24]=4)(=[O:22])=[O:21])[CH2:15]3)[C:11]=2[F:13])[C:6](=[O:34])[C:5]([C:35]([OH:37])=[O:36])=[CH:4]1)[CH3:2].Cl.[OH-].[Na+]>C(O)C>[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:33])=[C:10]([N:14]3[CH2:18][CH2:17][CH:16]([NH:19][S:20]([C:23]4[CH:24]=[CH:25][C:26]([NH2:29])=[CH:27][CH:28]=4)(=[O:22])=[O:21])[CH2:15]3)[C:11]=2[F:13])[C:6](=[O:34])[C:5]([C:35]([OH:37])=[O:36])=[CH:4]1)[CH3:2]
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 14798Sodium HydroxideHCID 189182031-Ethyl-6,8-difluoro-1,4-dihydro-4-oxo-7-[3-(4-acetamidobenzenesulfonamido)-1-pyrrolidinyl]-3-quinolinecarboxylic acid

生成物 1

HCID 189182091-Ethyl-6,8-difluoro-1,4-dihydro-4-oxo-7-[3-(4-aminobenzenesulfonamido)-1-pyrrolidinyl]-3-quinolinecarboxylic acid

試薬・触媒・溶媒 1

HCID 702
Ethanol
溶媒

実験手順

To the compound obtained in Example 14 is added a mixture solution made up of 100 ml of 2N hydrochloric acid and 10 ml of ethanol, and the resulting mixture is refluxed for 4 hours while heating. After cooling, the reaction mixture is neutralized with 2N sodium hydroxide solution and concentrated under reduced pressure. The residue is added to water which is then adjusted to pH 13 with 2N sodium hydroxide solution to dissolve, and any undissolved matter, if present, is removed. The solution is adjusted to pH 7 with acetic acid. Precipitating crystals are collected by filtration and washed. To the washed crystals is added water, pH adjusted to 3 to dissolve, and any undissolved matter, if present, is removed. The solution is then adjusted to pH 7 with 2N sodium hydroxide solution and precipitating crystals are collected by filtration and washed with water. Recrystallization from DMF-methanol gives 1.07 g of the titled compound. Melting point 214°-216° C.

後処理

  1. temperaturethe resulting mixture is refluxed for 4 hours
  2. temperaturewhile heating
  3. temperatureAfter cooling
  4. concentrationconcentrated under reduced pressure
  5. additionThe residue is added to water which
  6. dissolutionto dissolve
  7. customany undissolved matter, if present, is removed
  8. customPrecipitating crystals
  9. filtrationare collected by filtration
  10. washwashed
  11. additionTo the washed crystals is added water
  12. dissolutionto dissolve
  13. customany undissolved matter, if present, is removed
  14. customprecipitating crystals
  15. filtrationare collected by filtration
  16. washwashed with water
  17. customRecrystallization from DMF-methanol

出典と根拠

ORDレコード
ord-28aefd192dec4f92be9f004da9d82e1b
出典データセット
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05753658

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート