Diisopropylethylamine → Ofloxacin

HRID 1941532

反応式

HRID 1941532 の反応式
C(N1C2C(=CC(F)=C(F)C=2F)[C:6](=[O:16])C(C(O)=O)=C1)C.[C:20]([N:24]1[C:33]2[C:28](=[CH:29][C:30]([F:35])=[C:31](Cl)[N:32]=2)[C:27](=[O:36])[C:26]([C:37]([OH:39])=[O:38])=[CH:25]1)([CH3:23])([CH3:22])C.[CH:40]([N:43]([CH2:47]C)[CH:44](C)[CH3:45])(C)[CH3:41]>CO.C(Cl)Cl.CN(C=O)C>[F:35][C:30]1[C:31]([N:32]2[CH2:45][CH2:44][N:43]([CH3:47])[CH2:40][CH2:41]2)=[C:6]2[O:16][CH2:23][CH:20]([CH3:22])[N:24]3[CH:25]=[C:26]([C:37]([OH:39])=[O:38])[C:27](=[O:36])[C:28]([CH:29]=1)=[C:33]23

参加物

7

反応物 3

HCID 81531DiisopropylethylamineHCID 98351791-Ethyl-6,7,8-trifluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acidHCID 151890371-(Tert-butyl)-7-chloro-6-fluoro-1,4-dihydro-4-oxo-1,8-napthyridine-3-carboxylic acid

生成物 1

HCID 4583Ofloxacin

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 6228Dimethylformamide溶媒2 回HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of Compound 4 (1.9 g), prepared in the same manner as Compound 5 in Example 11, in a 1:1 mixture of DMF and CH2Cl2 (60 mL) is slowly added a solution of Compound 3 (2.32 g) in a 1:1 mixture of DMF and CH2Cl2 (30 mL), under N2. N,N-Diisopropylethylamine (0.98 mL) is added dropwise and the reaction is allowed to stir at ambient temperature until complete. Upon completion, methanol (15 mL) is added and the mixture is stirred for 15 minutes. The volatiles are removed in vacuo until a small mount of DMF remains whereupon methanol (150 mL) is added. The mixture is stirred for 5 minutes and filtered to obtain Compound 5.

後処理

  1. stirringthe mixture is stirred for 15 minutes
  2. customThe volatiles are removed in vacuo until a small mount of DMF
  3. additionis added
  4. stirringThe mixture is stirred for 5 minutes
  5. filtrationfiltered

出典と根拠

ORDレコード
ord-aa2162976f724c118f9bb8650ed5d929
出典データセット
uspto-grants-1997_12
特許番号
US05703231

関連ノート

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