Hydrochloric Acid → 4-[Benzo(B)thiophen-2-YL]benzoic acid

HRID 1096945ノート

反応式

HRID 1096945 の反応式
[OH-].[Na+].[S:3]1[C:7]([C:8]2[CH:17]=[CH:16][C:11]([C:12]([O:14]C)=[O:13])=[CH:10][CH:9]=2)=[CH:6][C:5]2[CH:18]=[CH:19][CH:20]=[CH:21][C:4]1=2.Cl>CO>[S:3]1[C:7]([C:8]2[CH:17]=[CH:16][C:11]([C:12]([OH:14])=[O:13])=[CH:10][CH:9]=2)=[CH:6][C:5]2[CH:18]=[CH:19][CH:20]=[CH:21][C:4]1=2

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 4137384Methyl 4-benzo[b]thien-2-ylbenzoate

生成物 1

HCID 41373834-[Benzo(B)thiophen-2-YL]benzoic acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Aqueous 5 N sodium hydroxide solution (0.28 mL, 1.40 mmol) was added to a methanol (2.3 mL) solution of methyl 4-(benzo[b]thiophen-2-yl)benzoate (124 mg, 0.462 mmol), and refluxed for 3 hours. After left cooled, 5 N hydrochloric acid (0.28 mL, 1.40 mmol) was added to the reaction mixture, and concentrated under reduced pressure. 20% methanol/THF was added to the residue, the mixture was filtered, and the filtrate was concentrated under reduced pressure. Diethyl ether was added to the residue, the insoluble matter was taken out through filtration, and dried to obtain the title compound as a pale yellow solid.

後処理

  1. temperaturerefluxed for 3 hours
  2. waitAfter left
  3. temperaturecooled
  4. concentrationconcentrated under reduced pressure
  5. addition20% methanol/THF was added to the residue
  6. filtrationthe mixture was filtered
  7. concentrationthe filtrate was concentrated under reduced pressure
  8. additionDiethyl ether was added to the residue
  9. filtrationthe insoluble matter was taken out through filtration
  10. customdried

出典と根拠

ORDレコード
ord-aceecb72c08044efa61324c70ee2de39
出典データセット
uspto-grants-2012_03
特許番号
US08138197B2

反応ノート

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