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

HRID 539209
ノート
印刷プレビュー

反応式

HRID 539209 の反応式
[N:1]1([C:7]2[CH:8]=[C:9]([C:20]([O-:22])=[O:21])[C:10]3[N:14]=[C:13]([C:15]([F:18])([F:17])[F:16])[NH:12][C:11]=3[CH:19]=2)[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[OH-].[Na+].[ClH:25].O1[CH2:30][CH2:29][CH2:28][CH2:27]1>CO.CS(C)=O>[Cl:25][C:28]1[C:29]([CH3:30])=[C:19]([CH2:11][N:12]2[C:11]3[CH:19]=[C:7]([N:1]4[CH2:2][CH2:3][O:4][CH2:5][CH2:6]4)[CH:8]=[C:9]([C:20]([OH:22])=[O:21])[C:10]=3[N:14]=[C:13]2[C:15]([F:17])([F:16])[F:18])[CH:7]=[CH:8][CH:27]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 1317319656-(4-morpholinyl)-2-(trifluoromethyl)-1H-benzimidazole-4-carboxylate

生成物 1

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

試薬・触媒・溶媒 2

HCID 679
Dimethyl Sulfoxide
溶媒
HCID 887Methanol溶媒

反応条件

温度
70 °C

実験手順

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]+.

後処理

  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)

出典と根拠

ORDレコード
ord-3c3b0dfeee694cf5b4c9097ac719f064
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08865912B2

反応ノート

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