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

HRID 248535노트

반응식

HRID 248535 반응식
[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

참가 물질

4

반응물 2

HCID 712FormaldehydeHCID 14839412HCID 14839412, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 284Formic Acid용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cc804431de034dc09cf9ccc7314c8cfb
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05210193

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