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Hydrochloric Acid → N-{4-[4-(4-Oxo-piperidin-1-yl)-phenylsulfamoyl]-phenyl}-acetamide

HRID 1794842
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HRID 1794842 반응식
O1[C:5]2([CH2:10][CH2:9][N:8]([C:11]3[CH:16]=[CH:15][C:14]([NH:17][S:18]([C:21]4[CH:26]=[CH:25][C:24]([NH:27][C:28](=[O:30])[CH3:29])=[CH:23][CH:22]=4)(=[O:20])=[O:19])=[CH:13][CH:12]=3)[CH2:7][CH2:6]2)[O:4]CC1.Cl>[OH-].[Na+]>[O:4]=[C:5]1[CH2:6][CH2:7][N:8]([C:11]2[CH:16]=[CH:15][C:14]([NH:17][S:18]([C:21]3[CH:26]=[CH:25][C:24]([NH:27][C:28](=[O:30])[CH3:29])=[CH:23][CH:22]=3)(=[O:19])=[O:20])=[CH:13][CH:12]=2)[CH2:9][CH2:10]1
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HCID 313Hydrochloric AcidHCID 22220392N-{4-[4-(1,4-Dioxa-8-aza-spiro[4.5]dec-8-yl)-phenylsulfamoyl]-phenyl}-acetamide

생성물 1

HCID 22220411N-{4-[4-(4-Oxo-piperidin-1-yl)-phenylsulfamoyl]-phenyl}-acetamide수율 60.7%

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

N-{4-[4-(1,4-Dioxa-8-aza-spiro[4.5]dec-8-yl)-phenylsulfamoyl]-phenyl}-acetamide (which was obtained in Example 215) (2.2 g, 5.1 mmol) was treated with concentrated hydrochloric acid (50 mL) at 0° C. and then allowed to warm to room temperature. After 30 min., ˜20 mL of 5 N NaOH was added dropwise and the precipitate was collected by filtration, and dried over P2O5 to give the title compound as a white solid (1.2 g); 1H NMR (300 MHz, DMSO-d6) δ 2.06 (s, 3 H), 2.43 (t, J=5.8 Hz, 4 H), 3.53 (t, J=5.8 Hz, 4 H), 6.85–7.05 (m, 4 H), 7.62 (d, J=9.0 Hz, 2 H), 7.71 (d, J=9.0 Hz, 2 H), 9.81 (s, 1 H), 10.35 (s, 1 H); MS (ES) m/z: 388.3 (MH+); HRMS Calcd. for C19H21N3O4S(M+):387.1253. Found: 387.1272.

후처리

  1. filtrationthe precipitate was collected by filtration
  2. dry with materialdried over P2O5

출처 및 근거

ORD 기록
ord-52308f05b72d4609bfbd0ceb767d219b
출처 데이터셋
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07022716B2

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