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Hydrochloric Acid → HCID 25254148、化合物

HRID 333776
ノート
印刷プレビュー

反応式

HRID 333776 の反応式
C[O:2][C:3](=[O:28])[CH2:4][O:5][C:6]1[CH:11]=[C:10]([C:12]([OH:27])([C:23]([F:26])([F:25])[F:24])[CH:13]([C:15]2[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][C:16]=2[Cl:22])[CH3:14])[CH:9]=[CH:8][N:7]=1.[OH-].[Na+].Cl>CO>[Cl:22][C:16]1[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:15]=1[CH:13]([CH3:14])[C:12]([C:10]1[CH:9]=[CH:8][N:7]=[C:6]([O:5][CH2:4][C:3]([OH:28])=[O:2])[CH:11]=1)([OH:27])[C:23]([F:25])([F:26])[F:24]
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

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 25254606{4-[2-(2,4-Dichloro-phenyl)-1-hydroxy-1-trifluoromethyl-propyl]-pyridin-2-yloxy}-acetic acid methyl ester

生成物 1

HCID 25254148HCID 25254148、化合物収率 78.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

反応条件

温度
55 °C

実験手順

To a solution of {4-[2-(2,4-dichloro-phenyl)-1-hydroxy-1-trifluoromethyl-propyl]-pyridin-2-yloxy}-acetic acid methyl ester (127 mg) in methanol (2 mL) was added an aqueous solution of NaOH (1N, 0.58 mL) and the mixture was allowed to stir at 55° C. for 2 hours. The pH of the mixture was adjusted to pH 2 with aqueous 1N HCl solution and methanol was removed by evaporation. The aqueous solution was extracted twice with ethyl acetate and the organic layers were washed with brine, dried and evaporated. The residual oil was stirred in hexane (5 mL) over night and the suspension was filtered to give the title compound as a colorless powder (96 mg). MS (m/e): 424.2 (MH)+.

後処理

  1. customwas removed by evaporation
  2. extractionThe aqueous solution was extracted twice with ethyl acetate
  3. washthe organic layers were washed with brine
  4. customdried
  5. customevaporated
  6. stirringThe residual oil was stirred in hexane (5 mL) over night
  7. filtrationthe suspension was filtered

出典と根拠

ORDレコード
ord-a50d9b3f1a80443ca6ceeaec97cd1a31
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08883786B2

反応ノート

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