2-[5-Chloro-3-(4-chloro-3-trifluoromethyl-benzenesulfonylamino)-pyridine-2-carbonyl]benzoic acid → 2-[5-Chloro-3-(4-chloro-3-trifluoromethyl-benzenesulfonylamino)-pyridine-2-carbonyl]benzoic acid methyl ester

HRID 419204ノート

反応式

HRID 419204 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([NH:19][S:20]([C:23]2[CH:28]=[CH:27][C:26]([Cl:29])=[C:25]([C:30]([F:33])([F:32])[F:31])[CH:24]=2)(=[O:22])=[O:21])[C:5]([C:8]([C:10]2[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=2[C:12]([OH:14])=[O:13])=[O:9])=[N:6][CH:7]=1.Cl.O1CCOC[CH2:36]1>CO>[CH3:36][O:13][C:12](=[O:14])[C:11]1[CH:15]=[CH:16][CH:17]=[CH:18][C:10]=1[C:8]([C:5]1[C:4]([NH:19][S:20]([C:23]2[CH:28]=[CH:27][C:26]([Cl:29])=[C:25]([C:30]([F:33])([F:32])[F:31])[CH:24]=2)(=[O:21])=[O:22])=[CH:3][C:2]([Cl:1])=[CH:7][N:6]=1)=[O:9]

参加物

4

反応物 2

HCID 116565312-[5-Chloro-3-(4-chloro-3-trifluoromethyl-benzenesulfonylamino)-pyridine-2-carbonyl]benzoic acidHCID 204431481,4-Dioxane hydrochloride

生成物 1

HCID 579420922-[5-Chloro-3-(4-chloro-3-trifluoromethyl-benzenesulfonylamino)-pyridine-2-carbonyl]benzoic acid methyl ester

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 2-[5-chloro-3-(4-chloro-3-trifluoromethyl-benzenesulfonylamino)-pyridine-2-carbonyl]benzoic acid (20 mg), 4N HCl/dioxane (1 mL) and 1.5 mL of methanol was refluxed overnight. After cooled to room temperature, the mixture was concentrated and the residue was diluted with ethyl acetate, washed with sodium bicarbonate and brine and dried. Removal of the solvents afforded the title compound as an off white solid: 1H NMR: (CDCl3, ppm) δ 11.20 (s, 1H), 8.22 (m, 2H), 8.04 (m, 2H), 7.94 (m, 1H), 7.62 (m, 2H), 7.54 (m, 1H), 7.31 (m, 1H), 3.54 (s, 3H); MS: (M+H)/z=533.0.

後処理

  1. temperaturewas refluxed overnight
  2. concentrationthe mixture was concentrated
  3. additionthe residue was diluted with ethyl acetate
  4. washwashed with sodium bicarbonate and brine
  5. customdried
  6. customRemoval of the solvents

出典と根拠

ORDレコード
ord-e270cd1d865345fb8a333eb9844facb9
出典データセット
uspto-grants-2012_01
特許番号
US08093247B2

反応ノート

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