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Hydrochloric Acid → 1-Cyclopropyl-8-(difluoromethoxy)-7-(1-methyl-2,3-dihydro-1H-isoindol-5-yl)-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

HRID 377294
ノート
印刷プレビュー

反応式

HRID 377294 の反応式
[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][CH:10]=[C:11]([C:18]4[CH:19]=[C:20]5[C:24](=[CH:25][CH:26]=4)[CH:23]([CH3:27])[N:22](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[CH2:21]5)[C:12]=3[O:14][CH:15]([F:17])[F:16])[C:7](=[O:47])[C:6]([C:48]([O:50]CC)=[O:49])=[CH:5]2)[CH2:3][CH2:2]1.Cl>C(O)C>[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][CH:10]=[C:11]([C:18]4[CH:19]=[C:20]5[C:24](=[CH:25][CH:26]=4)[CH:23]([CH3:27])[NH:22][CH2:21]5)[C:12]=3[O:14][CH:15]([F:17])[F:16])[C:7](=[O:47])[C:6]([C:48]([OH:50])=[O:49])=[CH:5]2)[CH2:3][CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 15887920HCID 15887920、化合物

生成物 1

HCID 4799301-Cyclopropyl-8-(difluoromethoxy)-7-(1-methyl-2,3-dihydro-1H-isoindol-5-yl)-4-oxo-1,4-dihydroquinoline-3-carboxylic acid収率 91.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

In 4 ml of ethanol was suspended 1.00 g of ethyl (-)-1-cyclopropyl-8-difluoromethoxy-7-(1-methyl-2-tritylisoindolin-5-yl)-1,4-dihydro-4-oxoquinoline-3-carboxylate, followed by adding thereto 0.26 ml of 6N hydrochloric acid, and the resulting mixture was stirred at room temperature for 30 minutes. The reaction mixture was filtered, after which 0.75 ml of a 5N aqueous sodium hydroxide solution was added to the filtrate and the resulting mixture was stirred at room temperature for 1 hour. To the reaction mixture was added 16 ml of water, followed by filtration. Carbon dioxide was bubbled into the filtrate and the crystals were collected by filtration to obtain 0.56 g of light-yellow (-)-1-cyclopropyl-8-difluoromethoxy-7-(1-methyl-isoindolin-5-yl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid.

後処理

  1. additionby adding
  2. filtrationThe reaction mixture was filtered
  3. additionafter which 0.75 ml of a 5N aqueous sodium hydroxide solution was added to the filtrate
  4. additionTo the reaction mixture was added 16 ml of water
  5. filtrationfollowed by filtration
  6. customCarbon dioxide was bubbled into the filtrate
  7. filtrationthe crystals were collected by filtration

出典と根拠

ORDレコード
ord-bbfbfb64f2184b60ad0af4256993f696
出典データセット
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06025370

反応ノート

読み込み中…

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