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 1721096ノート

反応式

HRID 1721096 の反応式
[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]

参加物

4

反応物 2

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

生成物 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

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
120 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2d135255379140d0a5d583e1f314736b
出典データセット
uspto-grants-1996_04
特許番号
US05508428

反応ノート

読み込み中…