Hydrochloric Acid → HCID 86655402、化合物

HRID 2190472ノート

反応式

HRID 2190472 の反応式
[CH3:1][C:2]([O:6][C:7]1[CH:8]=[C:9]([CH:14]=[CH:15][CH:16]=1)[C:10]([O:12]C)=[O:11])([CH3:5])[C:3]#[CH:4].CO.O.Cl>O1CCCC1>[CH3:5][C:2]([O:6][C:7]1[CH:8]=[C:9]([CH:14]=[CH:15][CH:16]=1)[C:10]([OH:12])=[O:11])([CH3:1])[C:3]#[CH:4]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 962WaterHCID 76333229Methyl 3-[(1,1-dimethylprop-2-yn-1-yl)oxy]benzoate

生成物 1

HCID 86655402HCID 86655402、化合物収率 101.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of methyl 3-[(1,1-dimethylprop-2-yn-1-yl)oxy]benzoate (4.0 g, 18.3 mmol) in tetrahydrofuran (10 mL) were added lithium hydroxide•monohydrate (865 mg, 20.6 mmol), methanol (10 mL) and water (5 mL), and the mixture was stirred at room temperature for 12 hr. The reaction mixture was adjusted to pH 3 by slowly adding 1N hydrochloric acid, and extracted with ethyl acetate (100 mL×2). The ethyl acetate layers were combined, and dried over anhydrous sodium sulfate. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure to give the title compound (3.8 g, 99%) as a colorless oil.

後処理

  1. extractionextracted with ethyl acetate (100 mL×2)
  2. dry with materialdried over anhydrous sodium sulfate
  3. filtrationThe insoluble material was filtered off
  4. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-2a1f052b16c740dd91986ce7ca1879c8
出典データセット
uspto-grants-2012_12
特許番号
US08324395B2

反応ノート

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