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Diethyl Ether → Ethyl 7-(3-aminopyrrolidin-1-yl)-1-(2,4-difluorophenyl)-6-fluoro-4-oxo-1,8-naphthyridine-3-carboxylate

HRID 246979
ノート
印刷プレビュー

反応式

HRID 246979 の反応式
Cl.Cl.[NH2:3][CH:4]1[CH2:8][CH2:7][NH:6][CH2:5]1.C(N(CC)CC)C.C1(S([C:24]2[N:33]=[C:32]3[C:27]([C:28](=[O:47])[C:29]([C:42]([O:44][CH2:45][CH3:46])=[O:43])=[CH:30][N:31]3[C:34]3[CH:39]=[CH:38][C:37]([F:40])=[CH:36][C:35]=3[F:41])=[CH:26][C:25]=2[F:48])=O)C=CC=CC=1.C(OCC)C>C(O)C>[NH2:3][CH:4]1[CH2:8][CH2:7][N:6]([C:24]2[N:33]=[C:32]3[C:27]([C:28](=[O:47])[C:29]([C:42]([O:44][CH2:45][CH3:46])=[O:43])=[CH:30][N:31]3[C:34]3[CH:39]=[CH:38][C:37]([F:40])=[CH:36][C:35]=3[F:41])=[CH:26][C:25]=2[F:48])[CH2:5]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 8471TriethylamineHCID 13849340Ethyl 7-benzenesulfinyl-1-(2,4-difluorophenyl)-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylateHCID 162125963-Aminopyrrolidine dihydrochloride

生成物 1

HCID 13667039Ethyl 7-(3-aminopyrrolidin-1-yl)-1-(2,4-difluorophenyl)-6-fluoro-4-oxo-1,8-naphthyridine-3-carboxylate収率 83.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

In 3 ml of ethanol was suspended 120 mg of 3-aminopyrrolidine dihydrochloride, and 250 mg of triethylamine was added thereto, after which 300 mg of ethyl 7-benzenesulfinyl-1-(2,4-difluorophenyl)-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylate was added thereto. The resulting mixture was subjected to reaction at room temperature for 3 hours, and to the reaction mixture was added 10 ml of diethyl ether, after which crystals were collected by filtration, and washed with 12 ml of water to obtain 230 mg (yield 83.8%) of ethyl 7-(3-amino-1-pyrrolidinyl)-1-(2,4-difluorophenyl)-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylate. The physical properties of this compound were identical with those of the compound obtained in Example 64.

後処理

  1. additionwas added
  2. customThe resulting mixture was subjected to reaction at room temperature for 3 hours
  3. filtrationafter which crystals were collected by filtration
  4. washwashed with 12 ml of water

出典と根拠

ORDレコード
ord-d7391d3c050e4d8c8a530440403e03ee
出典データセット
uspto-grants-1987_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04704459

反応ノート

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