Tert-butyl 5-azaspiro[2.4]heptan-7-ylcarbamate → 7-(7-Tert-butoxycarbonylamino-5-azaspiro[2,4]heptan-5-yl)-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

HRID 1975334노트

반응식

HRID 1975334 반응식
[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:15])=[C:11](F)[CH:12]=3)[C:7](=[O:16])[CH:6]([C:17]([OH:19])=[O:18])[CH2:5]2)[CH2:3][CH2:2]1.[C:20]([O:24][C:25]([NH:27][CH:28]1[C:32]2([CH2:34][CH2:33]2)[CH2:31][NH:30][CH2:29]1)=[O:26])([CH3:23])([CH3:22])[CH3:21]>CS(C)=O>[C:20]([O:24][C:25]([NH:27][CH:28]1[C:32]2([CH2:33][CH2:34]2)[CH2:31][N:30]([C:11]2[CH:12]=[C:13]3[C:8]([C:7](=[O:16])[C:6]([C:17]([OH:19])=[O:18])=[CH:5][N:4]3[CH:1]3[CH2:3][CH2:2]3)=[CH:9][C:10]=2[F:15])[CH2:29]1)=[O:26])([CH3:23])([CH3:21])[CH3:22]

참가 물질

4

반응물 2

HCID 14930995Tert-butyl 5-azaspiro[2.4]heptan-7-ylcarbamateHCID 151155821-Cyclopropyl-6,7-difluoro-2,3-dihydro-4-oxoquinoline-3-carboxylic acid

생성물 1

HCID 153380107-(7-Tert-butoxycarbonylamino-5-azaspiro[2,4]heptan-5-yl)-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
120 °C

실험 절차

250 mg of 1-cyclopropyl-6,7-difluoro-2,3-dihydro-4-oxoquinoline-3-carboxylic acid and 250 mg of compound 11 were added to 4 ml of dimethyl sulfoxide and the mixture was heated at 120° C. for 2 hours. After cooling, the solvent was removed under reduced pressure and the residue was crystallized by the addition of ethanol. The crystals were collected by filtration. The procedure gave 7-(7-tert-butoxycarbonylamino-5-azaspiro[2,4]heptan-5-yl)-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid as a crude product.

후처리

  1. temperatureAfter cooling
  2. customthe solvent was removed under reduced pressure
  3. customthe residue was crystallized by the addition of ethanol
  4. filtrationThe crystals were collected by filtration

출처 및 근거

ORD 기록
ord-85a72b319b7e4891bcc6273c1e335d9e
출처 데이터셋
uspto-grants-1994_02
특허 번호
US05286723

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