Methanol → 2-Chloro-3-(1-cyano-1-methylethyl)benzoic acid

HRID 1800702ノート

反応式

HRID 1800702 の反応式
[Cl:1][C:2]1[C:11]([C:12]([C:15]#[N:16])([CH3:14])[CH3:13])=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([O:6]C)=[O:5].CO.O.O.[OH-].[Li+]>O1CCCC1>[Cl:1][C:2]1[C:11]([C:12]([C:15]#[N:16])([CH3:14])[CH3:13])=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([OH:6])=[O:5]

参加物

6

反応物 4

HCID 887MethanolHCID 962WaterHCID 168937Lithium hydroxide, monohydrateHCID 67312408Methyl 2-chloro-3-(1-cyano-1-methylethyl)benzoate

生成物 1

HCID 668102752-Chloro-3-(1-cyano-1-methylethyl)benzoic acid収率 91.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of methyl 2-chloro-3-(1-cyano-1-methylethyl)benzoate (1.67 g, 7.02 mmol) in tetrahydrofuran (24 mL)/methanol (8 mL)/water (8 mL) was added lithium hydroxide-monohydrate (501 mg, 11.9 mmol), and the mixture was stirred at room temperature for 2 hr. The reaction mixture was concentrated under reduced pressure, and 6N hydrochloric acid (2.8 mL) was added dropwise to the residue. The precipitate was collected by filtration, and washed with water to give the title compound (1.43 g, 91%) as a white powder.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure, and 6N hydrochloric acid (2.8 mL)
  2. additionwas added dropwise to the residue
  3. filtrationThe precipitate was collected by filtration
  4. washwashed with water

出典と根拠

ORDレコード
ord-30f7642a9cc24c6487e1255607344a51
出典データセット
uspto-grants-2013_01
特許番号
US08344135B2

反応ノート

読み込み中…