Hydrochloric Acid → HCID 14652622、化合物

HRID 477833ノート

反応式

HRID 477833 の反応式
[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:24])=[C:10]([N:14]3[CH2:19][CH2:18][O:17][CH:16]([CH2:20][NH:21]C=O)[CH2:15]3)[C:11]=2[F:13])[C:6](=[O:25])[C:5]([C:26]([OH:28])=[O:27])=[CH:4]1)[CH3:2].[ClH:29].O>CO>[ClH:29].[NH2:21][CH2:20][CH:16]1[CH2:15][N:14]([C:10]2[C:11]([F:13])=[C:12]3[C:7]([C:6](=[O:25])[C:5]([C:26]([OH:28])=[O:27])=[CH:4][N:3]3[CH2:1][CH3:2])=[CH:8][C:9]=2[F:24])[CH2:19][CH2:18][O:17]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 146526021-Ethyl-6,8-difluoro-7-[2-(formylaminomethyl)morpholino]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

生成物 1

HCID 14652622HCID 14652622、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 500 mg of 1-ethyl-6,8-difluoro-7-[2-(formylaminomethyl)morpholino]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid, 1 ml of concentrated hydrochloric acid, 2 ml of water and 10 ml of methanol is refluxed for 1.5 hours. The reaction mixture is concentrated under reduced pressure. The obtained crystals are washed with acetone, collected by filtration and recrystallized from dimethylformamide to give 7-[2-(aminomethyl)morpholino]-1-ethyl-6,8-difluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid hydrochloride, melting at 276°-278° C. with decomposition.

後処理

  1. concentrationThe reaction mixture is concentrated under reduced pressure
  2. washThe obtained crystals are washed with acetone
  3. filtrationcollected by filtration
  4. customrecrystallized from dimethylformamide

出典と根拠

ORDレコード
ord-1875382aeec84616b2a292f5272f54b6
出典データセット
uspto-grants-1989_12
特許番号
US04889857

反応ノート

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