Ethanol → HCID 86743975、化合物

HRID 1090401ノート

反応式

HRID 1090401 の反応式
Cl.[NH2:2][OH:3].[OH-:4].[Na+].O=[C:7]1[CH2:11][CH2:10][CH:9]([C:12]2[CH:21]=[C:20]3[C:15]([C:16](=[O:25])[CH:17]=[CH:18][N:19]3[CH:22]3[CH2:24][CH2:23]3)=[CH:14][C:13]=2[F:26])[CH2:8]1.[CH2:27]([OH:29])C>O>[N:2](=[C:7]1[CH2:11][CH2:10][CH:9]([C:12]2[CH:21]=[C:20]3[C:15]([C:16](=[O:25])[C:17]([C:27]([OH:29])=[O:4])=[CH:18][N:19]3[CH:22]3[CH2:24][CH2:23]3)=[CH:14][C:13]=2[F:26])[CH2:8]1)[OH:3]

参加物

6

反応物 4

HCID 702EthanolHCID 14798Sodium Hydroxide2 回HCID 443297Hydroxyamine hydrochlorideHCID 86743976HCID 86743976、化合物

生成物 1

HCID 86743975HCID 86743975、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 3.8 g (55 mol) of hydroxylamine hydrochloride in 100 ml of water was neutralized by the addition of 55 ml (55 mmol) of 1.0 N sodium hydroxide. To this was added a suspension of 16.5 g (50 mmol) of 7-(3 oxocyclopentyl)-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxoquinoline acid in a mixture of 150 ml of ethanol and 50 ml (50 mmol) of 1.0 N sodium hydroxide. The reaction mixture was heated at 60° for 4 hours and then at room temperature overnight. The alcohol was removed in vacuo and the aqueous was acidified to pH 2.0 with 6.0 M hydrochloric acid. The solid was removed by filtration, washed with water, and dried in vacuo to give 16.1 g of the title compound.

後処理

  1. additionTo this was added
  2. temperatureThe reaction mixture was heated at 60° for 4 hours
  3. customat room temperature
  4. customovernight
  5. customThe alcohol was removed in vacuo
  6. customThe solid was removed by filtration
  7. washwashed with water
  8. customdried in vacuo

出典と根拠

ORDレコード
ord-316d74a3c11844919876d2d15535292a
出典データセット
uspto-grants-1992_01
特許番号
US05081254

反応ノート

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