Hydrochloric Acid → HCID 72714576, 화합물

HRID 57944노트

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HRID 57944 반응식
[OH:1][C:2]1([C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([N:22]3[C:30]4[CH:29]=[C:28]([C:31]5[CH:32]=[N:33][N:34]([CH3:36])[CH:35]=5)[N:27]=[CH:26][C:25]=4[CH:24]=[N:23]3)[N:17]=2)[CH2:8][CH2:7][CH2:6][N:5](C(OC(C)(C)C)=O)[CH2:4][CH2:3]1.Cl>CO>[CH3:36][N:34]1[CH:35]=[C:31]([C:28]2[N:27]=[CH:26][C:25]3[CH:24]=[N:23][N:22]([C:18]4[N:17]=[C:16]([C:2]5([OH:1])[CH2:8][CH2:7][CH2:6][NH:5][CH2:4][CH2:3]5)[CH:21]=[CH:20][CH:19]=4)[C:30]=3[CH:29]=2)[CH:32]=[N:33]1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 86707129tert-butyl 4-hydroxy-4-(6-(6-(1-methyl-1H-pyrazol-4-yl)-1H-pyrazolo[4,3-c]pyridin-1-yl)pyridin-2-yl)azepane-1-carboxylate

생성물 1

HCID 72714576HCID 72714576, 화합물수율 31%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of tert-butyl 4-hydroxy-4-(6-(6-(1-methyl-1H-pyrazol-4-yl)-1H-pyrazolo[4,3-c]pyridin-1-yl)pyridin-2-yl)azepane-1-carboxylate (200 mg, 0.41 mmol) in a solution of HCl in MeOH (2.0 M, 10 mL) was stirred at room temperature for 1 hour, which was monitored by LCMS. After completion of the reaction, the reaction mixture was concentrated under reduced pressure. The crude was purified by reverse phase preparative HPLC to afford 230 as a light yellow solid (30 mg, 31%). 1H NMR (500 MHz, CDCl3) δ (ppm) 9.06 (s, 1H), 8.85 (s, 1H), 8.26 (s, 1H), 8.06 (s, 1H), 8.03 (s, 1H), 7.88-7.89 (d, J=4.5 Hz, 2H), 7.56-7.58 (t, J=9 Hz, 1H), 4.00 (s, 3H), 3.31-3.38 (m, 2H), 3.10-3.13 (t, J=13 Hz, 1H), 2.81-2.83 (t, J=12 Hz, 1H), 2.37-2.46 (m, 3H), 2.10-2.17 (m, 4H), 1.82-1.85 (t, J=14.5 Hz, 1H); MS (ESI) m/z: 390 [M+H]+.

후처리

  1. customAfter completion of the reaction
  2. concentrationthe reaction mixture was concentrated under reduced pressure
  3. customThe crude was purified by reverse phase preparative HPLC

출처 및 근거

ORD 기록
ord-ed9aeb3bd52f4c3f8eb1694e75482b26
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434725B2

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