Hydrochloric Acid → 1-[2-Fluoro-4-(2-{[4-(4-methylpiperazin-1-yl)piperidine-1-carbonyl]amino}piperidin-4-yloxy)phenylcarbamoyl]cyclopropanecarboxylic acid benzyl ester trihydrochloride

HRID 1712668노트

반응식

HRID 1712668 반응식
[CH2:1]([O:8][C:9]([C:11]1([C:14](=[O:46])[NH:15][C:16]2[CH:21]=[CH:20][C:19]([O:22][CH:23]3[CH2:28][CH2:27][NH:26][CH:25]([NH:29][C:30]([N:32]4[CH2:37][CH2:36][CH:35]([N:38]5[CH2:43][CH2:42][N:41]([CH3:44])[CH2:40][CH2:39]5)[CH2:34][CH2:33]4)=[O:31])[CH2:24]3)=[CH:18][C:17]=2[F:45])[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:47]>C(OCC)(=O)C>[ClH:47].[ClH:47].[ClH:47].[CH2:1]([O:8][C:9]([C:11]1([C:14](=[O:46])[NH:15][C:16]2[CH:21]=[CH:20][C:19]([O:22][CH:23]3[CH2:28][CH2:27][NH:26][CH:25]([NH:29][C:30]([N:32]4[CH2:37][CH2:36][CH:35]([N:38]5[CH2:39][CH2:40][N:41]([CH3:44])[CH2:42][CH2:43]5)[CH2:34][CH2:33]4)=[O:31])[CH2:24]3)=[CH:18][C:17]=2[F:45])[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 68496027HCID 68496027, 화합물

생성물 1

HCID 684981621-[2-Fluoro-4-(2-{[4-(4-methylpiperazin-1-yl)piperidine-1-carbonyl]amino}piperidin-4-yloxy)phenylcarbamoyl]cyclopropanecarboxylic acid benzyl ester trihydrochloride

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

1-[2-Fluoro-4-(2-{[4-(4-methylpiperazin-1-yl)piperidine-1-carbonyl]amino}piperidin-4-yloxy)phenylcarbamoyl]cyclopropanecarboxylic acid benzyl ester (189 mg) was dissolved in ethyl acetate (6 ml), and 4N hydrochloric acid in ethyl acetate (0.3 ml) was added. The resultant mixture was concentrated under reduced pressure, and methanol (0.5 ml) and ethyl acetate (4 ml) was added. The precipitate obtained by filtration was hygroscopic, thus it was collected using methanol (10 ml). The collected solution was again concentrated under reduced pressure, and methanol (0.5 ml) and tert-butyl methyl ether (4 ml) was added. The precipitate was filtered to give the title compound (102 mg).

후처리

  1. concentrationThe resultant mixture was concentrated under reduced pressure, and methanol (0.5 ml) and ethyl acetate (4 ml)
  2. additionwas added
  3. customThe precipitate obtained by filtration
  4. customthus it was collected
  5. concentrationThe collected solution was again concentrated under reduced pressure, and methanol (0.5 ml) and tert-butyl methyl ether (4 ml)
  6. additionwas added
  7. filtrationThe precipitate was filtered

출처 및 근거

ORD 기록
ord-43c58f0ff08b4ee7afdbf314b16e1f31
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07790885B2

반응 노트

불러오는 중…