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Acetic Acid → (S)-5-(4-(1-(2-(3-(difluoromethyl)-4,4,7,7-tetrafluoro-4,5,6,7-tetrahydro-1H-indazol-1-yl)acetamido)-2-(3,5-difluorophenyl)ethyl)-2-(4-hydroxypiperidin-1-yl)pyrimidin-5-yl)-2-fluorobenzamide

HRID 2170343
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HRID 2170343 반응식
[F:1][CH:2]([F:53])[C:3]1[C:11]2[C:10]([F:13])([F:12])[CH2:9][CH2:8][C:7]([F:15])([F:14])[C:6]=2[N:5]([CH2:16][C:17]([NH:19][C@H:20]([C:30]2[C:35]([C:36]3[CH:37]=[CH:38][C:39]([F:45])=[C:40]([CH:44]=3)[C:41]([NH2:43])=[O:42])=[CH:34][N:33]=[C:32]([N:46]3[CH2:51][CH2:50][C:49](=[O:52])[CH2:48][CH2:47]3)[N:31]=2)[CH2:21][C:22]2[CH:27]=[C:26]([F:28])[CH:25]=[C:24]([F:29])[CH:23]=2)=[O:18])[N:4]=1.C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].CCOC(C)=O>ClCCCl.O>[F:53][CH:2]([F:1])[C:3]1[C:11]2[C:10]([F:12])([F:13])[CH2:9][CH2:8][C:7]([F:14])([F:15])[C:6]=2[N:5]([CH2:16][C:17]([NH:19][C@H:20]([C:30]2[C:35]([C:36]3[CH:37]=[CH:38][C:39]([F:45])=[C:40]([CH:44]=3)[C:41]([NH2:43])=[O:42])=[CH:34][N:33]=[C:32]([N:46]3[CH2:47][CH2:48][CH:49]([OH:52])[CH2:50][CH2:51]3)[N:31]=2)[CH2:21][C:22]2[CH:27]=[C:26]([F:28])[CH:25]=[C:24]([F:29])[CH:23]=2)=[O:18])[N:4]=1
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참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 8857Ethyl AcetateHCID 5049666Sodium triacetoxyborohydrideHCID 90281442(S)-5-(4-(1-(2-(3-(difluoromethyl)-4,4,7,7-tetrafluoro-4,5,6,7-tetrahydro-1H-indazol-1-yl)acetamido)-2-(3,5-difluorophenyl)ethyl)-2-(4-oxopiperidin-1-yl)pyrimidin-5-yl)-2-fluorobenzamide

생성물 1

HCID 90281234
(S)-5-(4-(1-(2-(3-(difluoromethyl)-4,4,7,7-tetrafluoro-4,5,6,7-tetrahydro-1H-indazol-1-yl)acetamido)-2-(3,5-difluorophenyl)ethyl)-2-(4-hydroxypiperidin-1-yl)pyrimidin-5-yl)-2-fluorobenzamide

시약·촉매·용매 2

HCID 111,2-Dichloroethane용매HCID 962Water용매

실험 절차

To a solution of compound 19C (18 mg, 0.023 mmol) in 1,2-dichloroethane (0.5 ml), was added acetic acid (13 μL, 0.23 mmol) and sodium triacetoxyborohydride (9.7 mg, 0.046 mmol) at room temperature. After being stirred for 3 hours, the mixture was treated with EtOAc (10 mL) and water (3 mL). The organic layer was washed with brine (2 mL), dried (MgSO4), filtered, and concentrated under reduced pressure to furnish the crude product. This material was purified on reverse phase HPLC eluting with acetonitrile and water (with 0.1% TFA) to afford the title product. 1H NMR (400 MHz, CD3OD) δ 8.71 (d, J=8.5 Hz, 1H), 8.09 (s, 1H), 7.41 (dd, J=7.0, 2.3 Hz, 1H), 7.33 (m, 1H), 7.20 (dd, J=10.8, 8.5 Hz, 1H), 6.97-6.61 (m, 3H), 6.42 (d, J=6.2 Hz, 2H), 5.24 (t, J=7.2 Hz, 1H), 5.13-4.96 (m, 2H), 4.51 (m, 2H), 4.01-3.83 (m, 1H), 3.42 (m, 2H), 3.14-2.82 (m, 2H), 2.50 (m, 4H), 2.08-1.84 (m, 2H), 1.68-1.37 (m, 2H); MS (m/z) 756.22 [M+H]+.

후처리

  1. washThe organic layer was washed with brine (2 mL)
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customto furnish the crude product
  6. customThis material was purified on reverse phase HPLC
  7. washeluting with acetonitrile and water (with 0.1% TFA)

출처 및 근거

ORD 기록
ord-14fa772ee9c74f62966547579408c778
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09050344B2

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