Hydrochloric Acid → [3-(2-Formyl-4-trifluoromethyl-phenoxy)-phenyl]-acetic acid methyl ester

HRID 1969040ノート

反応式

HRID 1969040 の反応式
[CH3:1][O:2][C:3](=[O:27])[CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([O:11][C:12]2[CH:17]=[CH:16][C:15]([C:18]([F:21])([F:20])[F:19])=[CH:14][C:13]=2[CH:22](OC)[O:23]C)[CH:6]=1.Cl.CCOC(C)=O.O>C1COCC1>[CH3:1][O:2][C:3](=[O:27])[CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([O:11][C:12]2[CH:17]=[CH:16][C:15]([C:18]([F:19])([F:21])[F:20])=[CH:14][C:13]=2[CH:22]=[O:23])[CH:6]=1

参加物

6

反応物 4

HCID 313Hydrochloric Acid2 回HCID 962WaterHCID 8857Ethyl AcetateHCID 58237632[3-(2-Dimethoxymethyl-4-trifluoromethyl-phenoxy)-phenyl]-acetic acid methyl ester

生成物 1

HCID 58237636[3-(2-Formyl-4-trifluoromethyl-phenoxy)-phenyl]-acetic acid methyl ester

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
70 °C

実験手順

[3-(2-Dimethoxymethyl-4-trifluoromethyl-phenoxy)-phenyl]-acetic acid methyl ester (0.479 g, 1.42 mmol) and hydrogen chloride (4N in 1,4-dioxane; 1.5 mL, 6.0 mmol) were combined in THF (4 mL) and stirred at 70° C. for 1 hour. Some starting material was still seen by analytical LCMS, so additional hydrogen chloride (4N in 1,4-dioxane; 0.5 mL) was added, and the reaction was stirred for another hour at 70° C. After cooling to room temperature, the mixture was worked up with EtOAc and H2O, and the combined organic layers were dried and concentrated to give the title compound.

後処理

  1. additionwas added
  2. stirringthe reaction was stirred for another hour at 70° C
  3. temperatureAfter cooling to room temperature
  4. customthe combined organic layers were dried
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-63b98c6bcc824c08a43cf9e05ff07a0d
出典データセット
uspto-grants-2013_04
特許番号
US08426449B2

反応ノート

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