Formaldehyde → 1-Cyclopropyl-7-(3-cyclopropyl-4-methyl-1-piperazinyl)-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid

HRID 2165700ノート

反応式

HRID 2165700 の反応式
[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:23])=[C:11]([N:14]4[CH2:19][CH2:18][NH:17][CH:16]([CH:20]5[CH2:22][CH2:21]5)[CH2:15]4)[CH:12]=3)[C:7](=[O:24])[C:6]([C:25]([OH:27])=[O:26])=[CH:5]2)[CH2:3][CH2:2]1.[CH2:28]=O>C(O)=O>[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:23])=[C:11]([N:14]4[CH2:19][CH2:18][N:17]([CH3:28])[CH:16]([CH:20]5[CH2:21][CH2:22]5)[CH2:15]4)[CH:12]=3)[C:7](=[O:24])[C:6]([C:25]([OH:27])=[O:26])=[CH:5]2)[CH2:2][CH2:3]1

参加物

4

反応物 2

HCID 712FormaldehydeHCID 14839412HCID 14839412、化合物

生成物 1

HCID 230429671-Cyclopropyl-7-(3-cyclopropyl-4-methyl-1-piperazinyl)-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

反応条件

温度
100 °C

実験手順

A mixture of 210 mg of 1-cyclopropyl-7-(3-cyclopropyl-1-piperazinyl)-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid, 0.24 ml of 37% formaldehyde and 0.30 ml of 90% formic acid was heated at 100° C. for 4 hours, then allowed to cool and the excess reagents removed under reduced pressure. Water was added and the pH adjusted to 7 with 1N sodium hydroxide. The mixture was then extracted several times with chloroform:methanol (95:5), the extracts combined, dried, filtered and evaporated. The resulting oil was triturated with ether, giving 170 mg of the desired product.

後処理

  1. temperatureto cool
  2. customthe excess reagents removed under reduced pressure
  3. additionWater was added
  4. extractionThe mixture was then extracted several times with chloroform:methanol (95:5)
  5. customdried
  6. filtrationfiltered
  7. customevaporated
  8. customThe resulting oil was triturated with ether

出典と根拠

ORDレコード
ord-73de8de8b51f4d6db5ed75b68372bfd1
出典データセット
uspto-grants-1990_07
特許番号
US04940710

反応ノート

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