Hydrochloric Acid → HCID 68907622, 화합물

HRID 1510347노트

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HRID 1510347 반응식
[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

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 15604366HCID 15604366, 화합물

생성물 1

HCID 68907622HCID 68907622, 화합물수율 69%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-35a1ccec0aaf47c3855a95ed3574e80e
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08211910B2

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