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Hydrochloric Acid → 1-Cyclopropyl-6,8-difluoro-7-[2-(dimethylaminomethyl)morpholino]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid.hydrochloride

HRID 477863
ノート
印刷プレビュー

反応式

HRID 477863 の反応式
[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:25])=[C:11]([N:15]4[CH2:20][CH2:19][O:18][CH:17]([CH2:21][N:22]([CH3:24])[CH3:23])[CH2:16]4)[C:12]=3[F:14])[C:7](=[O:26])[C:6]([C:27]([O:29]CC)=[O:28])=[CH:5]2)[CH2:3][CH2:2]1.[ClH:32]>O.C(O)C>[ClH:32].[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:25])=[C:11]([N:15]4[CH2:20][CH2:19][O:18][CH:17]([CH2:21][N:22]([CH3:24])[CH3:23])[CH2:16]4)[C:12]=3[F:14])[C:7](=[O:26])[C:6]([C:27]([OH:29])=[O:28])=[CH:5]2)[CH2:2][CH2:3]1
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 2

HCID 313Hydrochloric AcidHCID 14652597Ethyl 1-cyclopropyl-6,8-difluoro-7-[2-(dimethylaminomethyl)morpholino]-1,4-dihydro-4-oxoquinoline-3-carboxylate

生成物 1

HCID 146525981-Cyclopropyl-6,8-difluoro-7-[2-(dimethylaminomethyl)morpholino]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid.hydrochloride収率 80%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒
HCID 962
Water
溶媒

実験手順

A solution of 2.21 g of ethyl 1-cyclopropyl-6,8-difluoro-7-[2-(dimethylaminomethyl)morpholino]-1,4-dihydro-4-oxoquinoline-3-carboxylate and 5 ml of concentrated hydrochloric acid in 10 ml of water and 10 ml of ethanol is refluxed, for 2.5 hours. The resultant mixture is concentrated under reduced pressure and to the obtained crystals is added ethanol. The crystals are filtered off with suction, washed with ethanol and then dried to give 1.82 g of 1-cyclopropyl-6,8-difluoro-7-[2-(dimethylaminomethyl)morpholino]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid.hydrochloride in 80% yield, melting at 267°-268° C.

後処理

  1. concentrationThe resultant mixture is concentrated under reduced pressure and to the obtained crystals
  2. additionis added ethanol
  3. filtrationThe crystals are filtered off with suction
  4. washwashed with ethanol
  5. customdried

出典と根拠

ORDレコード
ord-af4e4df0f73c4cb598a1039574a1f1f3
出典データセット
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04889857

反応ノート

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