Diisopropylethylamine → Ofloxacin

HRID 1941532

반응식

HRID 1941532 반응식
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

참가 물질

7

반응물 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

생성물 1

HCID 4583Ofloxacin

시약·촉매·용매 3

HCID 887Methanol용매HCID 6228Dimethylformamide용매2회HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-aa2162976f724c118f9bb8650ed5d929
출처 데이터셋
uspto-grants-1997_12
특허 번호
US05703231

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