Hydrochloric Acid → HCID 68907622、化合物

HRID 1510347ノート

反応式

HRID 1510347 の反応式
[NH2:1][C:2]1([CH3:30])[C:6]2([CH2:8][CH2:7]2)[CH2:5][N:4]([C:9]2[C:18]([O:19][CH3:20])=[C:17]3[C:12]([C:13](=[O:28])[C:14]([C:25]([OH:27])=[O:26])=[CH:15][N:16]3[C@@H:21]3[CH2:23][C@@H:22]3[F:24])=[CH:11][C:10]=2[F:29])[CH2:3]1.[ClH:31].C(O)(C)C>CO>[ClH:31].[NH2:1][C:2]1([CH3:30])[C:6]2([CH2:7][CH2:8]2)[CH2:5][N:4]([C:9]2[C:18]([O:19][CH3:20])=[C:17]3[C:12]([C:13](=[O:28])[C:14]([C:25]([OH:27])=[O:26])=[CH:15][N:16]3[C@@H:21]3[CH2:23][C@@H:22]3[F:24])=[CH:11][C:10]=2[F:29])[CH2:3]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 15604366HCID 15604366、化合物

生成物 1

HCID 68907622HCID 68907622、化合物収率 69%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

7-[7-amino-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 amino group in the substituent at position 7 is the same as the one produced in Example 9 (18.07 g, 39.4 mmol) was suspended in methanol (54 mL), and 1N hydrochloric acid (43.4 mL, 43.4 mmol) was added to the suspension at room temperature. Isopropyl alcohol (180 mL) was then added, and the mixture was stirred in a water bath at 50° C. for some time until precipitated gummy material thoroughly turned to crystal. After allowing to stand at room temperature for 1 hour, the crystals were collected by filtration, and washed with a small amount of isopropyl alcohol (twice). The crystals were then dried under reduced pressure to obtain the title compound 12.91 g (27.2 mmol, 69%) as a yellow powder.

後処理

  1. customuntil precipitated gummy material
  2. filtrationthe crystals were collected by filtration
  3. washwashed with a small amount of isopropyl alcohol (twice)
  4. customThe crystals were then dried under reduced pressure

出典と根拠

ORDレコード
ord-35a1ccec0aaf47c3855a95ed3574e80e
出典データセット
uspto-grants-2012_07
特許番号
US08211910B2

反応ノート

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