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Hydrochloric Acid → 1-[(3-chloro-2-methylphenyl)methyl]-6-(4-morpholinyl)-2-(trifluoromethyl)-1H-benzimidazole-4-carboxylic acid

HRID 1188829
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HRID 1188829 반응식
[Cl:1][C:2]1[C:3]([CH3:32])=[C:4]([CH2:8][N:9]2[C:13]3[CH:14]=[C:15]([N:22]4[CH2:27][CH2:26][O:25][CH2:24][CH2:23]4)[CH:16]=[C:17]([C:18]([O:20]C)=[O:19])[C:12]=3[N:11]=[C:10]2[C:28]([F:31])([F:30])[F:29])[CH:5]=[CH:6][CH:7]=1.[OH-].[Na+].Cl>CO.O1CCCC1.CS(C)=O>[Cl:1][C:2]1[C:3]([CH3:32])=[C:4]([CH2:8][N:9]2[C:13]3[CH:14]=[C:15]([N:22]4[CH2:23][CH2:24][O:25][CH2:26][CH2:27]4)[CH:16]=[C:17]([C:18]([OH:20])=[O:19])[C:12]=3[N:11]=[C:10]2[C:28]([F:31])([F:29])[F:30])[CH:5]=[CH:6][CH:7]=1
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참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 56960264methyl 1-[(3-chloro-2-methylphenyl)methyl]-6-(4-morpholinyl)-2-(trifluoromethyl)-1H-benzimidazole-4-carboxylate

생성물 1

HCID 569604001-[(3-chloro-2-methylphenyl)methyl]-6-(4-morpholinyl)-2-(trifluoromethyl)-1H-benzimidazole-4-carboxylic acid

시약·촉매·용매 3

HCID 679Dimethyl Sulfoxide
용매
HCID 887Methanol용매
HCID 8028Tetrahydrofuran용매

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온도
70 °C

실험 절차

A suspension of methyl 1-[(3-chloro-2-methylphenyl)methyl]-6-(4-morpholinyl)-2-(trifluoromethyl)-1H-benzimidazole-4-carboxylate, prepared as described in Example 49 (1.09 g, 2.330 mmol) in Methanol (12 mL) and Tetrahydrofuran (THF) (4 mL) was treated with 1 M aq. sodium hydroxide (12 mL, 12.00 mmol) and stirred at 70° C. for 1.5 h (mixture turned homogeneous). The reaction was cooled to room temperature, the volume reduced to half and the residue was acidified (pH 4) by the addition of 1 N HCl. The precipitate was collected, washed with water and dried to give crude desired product (918.6 mg, 2.024 mmol, 87% yield) as a yellow solid. A portion of it (140 mg) was suspended in 3.5 mL of DMSO. After sonication and heating, the solid went into solution but it crashed out. The precipitate was collected and washed with DMSO, but it still showed impurities by LC/MS. Another aliquot (132 mg) was dissolved with heating in 5 mL of DMSO and purified by reverse phase-HPLC (15 to 95% AcCN in water plus 0.1% TFA). The desired product was isolated by evaporation of the organic solvent: the precipitate was collected by filtration, washed with water and dried in a vacuum oven to afford pure desired product (89 mg, 0.192 mmol, 8.25% yield). 1H NMR (400 MHz, DMSO-d6) δ ppm 13.09 (s, 1H), 7.63 (d, J=2.27 Hz, 1H), 7.36 (d, J=7.83 Hz, 1H), 7.30 (d, J=2.27 Hz, 1H), 7.05 (t, J=7.96 Hz, 1H), 5.98 (d, J=7.58 Hz, 1H), 5.70 (s, 2H), 3.66-3.83 (m, 4H), 3.08-3.24 (m, 4H), 2.47 (s, 3H). MS (ES+) m/e 453.9 [M+H]+.

후처리

  1. customprepared
  2. temperatureThe reaction was cooled to room temperature
  3. customThe precipitate was collected
  4. washwashed with water
  5. customdried
  6. customto give crude desired product (918.6 mg, 2.024 mmol, 87% yield) as a yellow solid
  7. customAfter sonication
  8. temperatureheating
  9. customThe precipitate was collected
  10. washwashed with DMSO, but it still showed impurities by LC/MS
  11. dissolutionAnother aliquot (132 mg) was dissolved
  12. temperaturewith heating in 5 mL of DMSO
  13. custompurified by reverse phase-HPLC (15 to 95% AcCN in water plus 0.1% TFA)

출처 및 근거

ORD 기록
ord-a5f6c0f72d1b4a0c885a1f4a7f59fa2f
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08674090B2

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