Hydrochloric Acid → HCID 68907622、化合物

HRID 1510348ノート

反応式

HRID 1510348 の反応式
C(OC([NH:8][C:9]1([CH3:37])[C:13]2([CH2:15][CH2:14]2)[CH2:12][N:11]([C:16]2[C:25]([O:26][CH3:27])=[C:24]3[C:19]([C:20](=[O:35])[C:21]([C:32]([OH:34])=[O:33])=[CH:22][N:23]3[C@@H:28]3[CH2:30][C@@H:29]3[F:31])=[CH:18][C:17]=2[F:36])[CH2:10]1)=O)(C)(C)C.[ClH:38]>C(O)(C)C>[ClH:38].[NH2:8][C:9]1([CH3:37])[C:13]2([CH2:14][CH2:15]2)[CH2:12][N:11]([C:16]2[C:25]([O:26][CH3:27])=[C:24]3[C:19]([C:20](=[O:35])[C:21]([C:32]([OH:34])=[O:33])=[CH:22][N:23]3[C@@H:28]3[CH2:30][C@@H:29]3[F:31])=[CH:18][C:17]=2[F:36])[CH2:10]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 57758693HCID 57758693、化合物

生成物 1

HCID 68907622HCID 68907622、化合物収率 92%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒2 回

反応条件

温度
55 °C

実験手順

7-[7-(tert-Butoxycarbonylamino)-7-methyl-5-azaspiro[2.4]heptan-5-yl]-6-fluoro-1-[(1R,2S)-2-fluorocyclopropyl]-8-methoxy-1,4-dihydro-4-oxoquinoline-3-carboxylic acid in which configuration of the tert -butoxycarbonylamino group in the substituent at position 7 is the same as the one produced in Example 9 (267.2 g) was suspended in isopropyl alcohol (1.6 L), and 6N hydrochloric acid (405 mL, 2.43 mol) was added to the suspension while the suspension was stirred in an oil bath at 55° C. The mixture was stirred at the same temperature for 3.5 hours, and after allowing to cool to room temperature, isopropyl alcohol (2.4 L) was added. The reaction vessel was cooled in a water bath at 5° C., and the mixture was stirred at the same temperature for 13 hours. The precipitated crystals were collected by filtration and after air drying for several hours, the crystals were dried under reduced pressure at 40° C. to obtain 223.3 g (471 mmol, 92%) of the target compound as a yellow powder.

後処理

  1. stirringThe mixture was stirred at the same temperature for 3.5 hours
  2. temperatureto cool to room temperature
  3. temperatureThe reaction vessel was cooled in a water bath at 5° C.
  4. stirringthe mixture was stirred at the same temperature for 13 hours
  5. filtrationThe precipitated crystals were collected by filtration
  6. customafter air drying for several hours
  7. customthe crystals were dried under reduced pressure at 40° C.

出典と根拠

ORDレコード
ord-d89671350f0b4e24a6d02f785272ff43
出典データセット
uspto-grants-2012_07
特許番号
US08211910B2

反応ノート

読み込み中…