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Pyridine → HCID 23516247, 화합물

HRID 1793000
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HRID 1793000 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([I:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]1[C:18]([F:19])=[C:17]([F:20])[CH:16]=[CH:15][C:11]=1[C:12]([OH:14])=[O:13].N1C=CC=CC=1.FC(F)(F)C(O[C:32]1[C:37]([F:38])=[C:36]([F:39])[C:35]([F:40])=[C:34]([F:41])[C:33]=1[F:42])=O>CN(C)C=O.C(OCC)(=O)C>[F:38][C:37]1[C:32]([O:13][C:12](=[O:14])[C:11]2[CH:15]=[CH:16][C:17]([F:20])=[C:18]([F:19])[C:10]=2[NH:9][C:3]2[CH:4]=[CH:5][C:6]([I:8])=[CH:7][C:2]=2[Cl:1])=[C:33]([F:42])[C:34]([F:41])=[C:35]([F:40])[C:36]=1[F:39]
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참가 물질

6

반응물 3

HCID 1049PyridineHCID 4327891Pentafluorophenyl TrifluoroacetateHCID 10112191Zapnometinib2회

생성물 1

HCID 23516247HCID 23516247, 화합물수율 91%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate
용매

실험 절차

To a solution of the product of Example 2, Step A, 2-(2-chloro-4-iodophenylamino)-3,4-difluorobenzoic acid (10.0 g, 24.4 mmol), and pyridine (2.16 mL, 26.8 mmol) in anhydrous dimethylformamide (49 mL) was added pentafluorophenyl trifluoroacetate (5.35 mL, 30.5 mmol). The resultant solution was stirred at ambient temperature for 2 hours. The reaction mixture was diluted with ethyl acetate (600 mL) and washed with 0.1 M aqueous hydrochloric acid (2×240 mL), 25% saturated aqueous sodium bicarbonate (2×240 mL), and saturated brine (240 mL). The organics were dried over anhydrous magnesium sulfate and concentrated under reduced pressure to afford an oil that was purified on silica gel. Elution with hexanes-ethyl acetate (19:1) afforded 2-(2-chloro-4-iodophenylamino)-3,4-difluorobenzoic acid pentafluorophenyl ester (12.8 g, 91%) as a pale-yellow powder: m.p. 108.5–110.0° C.; 1H-NMR (400 MHz, CDCl3) δ 8.77 (br s, 1 H), 8.07 (br s, 1 H), 7.69 (br s, 1 H), 7.48 (br d, J=7.0 Hz, 1 H), 6.91 (br d, J=7.2 Hz, 1 H), 6.67 (br s., 1 H); 19F-NMR (376 MHz, CDCl3) δ −123.74 (s, 1F), −139.17 (d, J=16.8 Hz, 1F), −152.35 (d, J=21.4 Hz, 2F), −156.96 (t, J=21.4 Hz, 1F), −161.81 (t, J=21.4 Hz, 2F). Anal. Calcd/found for C19H6NO2F7ClI: C, 39.65/39.32; H, 1.05/0.91; N, 2.43/2.35; F, 23.10/22.85; Cl, 6.16/6.92; I, 22.05/22.50.

후처리

  1. washwashed with 0.1 M aqueous hydrochloric acid (2×240 mL), 25% saturated aqueous sodium bicarbonate (2×240 mL), and saturated brine (240 mL)
  2. dry with materialThe organics were dried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customto afford an oil that
  5. customwas purified on silica gel
  6. washElution with hexanes-ethyl acetate (19:1)

출처 및 근거

ORD 기록
ord-899d1d4e9b5d4a96af3a362160180f80
출처 데이터셋
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07078438B2

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