Lithium Hydroxide → HCID 58046316、化合物

HRID 2359306ノート

反応式

HRID 2359306 の反応式
[Cl:1][C:2]1[CH:21]=[CH:20][C:5]([O:6][C:7]2[CH:16]=[CH:15][C:10]([C:11]([O:13]C)=[O:12])=[C:9]([CH2:17][O:18][CH3:19])[CH:8]=2)=[CH:4][C:3]=1[C:22]([F:25])([F:24])[F:23].[OH-].[Li+]>O1CCCC1.O.C(OCC)(=O)C>[Cl:1][C:2]1[CH:21]=[CH:20][C:5]([O:6][C:7]2[CH:16]=[CH:15][C:10]([C:11]([OH:13])=[O:12])=[C:9]([CH2:17][O:18][CH3:19])[CH:8]=2)=[CH:4][C:3]=1[C:22]([F:23])([F:24])[F:25]

参加物

6

反応物 2

HCID 3939Lithium Hydroxide2 回HCID 58046348Benzoic acid, 4-[4-chloro-3-(trifluoromethyl)phenoxy]-2-(methoxymethyl)-, methyl ester

生成物 1

HCID 58046316HCID 58046316、化合物収率 100%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of methyl 4-[4-chloro-3-(trifluoromethyl)phenoxy]-2-(methoxymethyl)benzoate (Preparation 34, 0.140 g, 0.000374 mol) in tetrahydrofuran (3.00 mL) and water (3.00 mL) was added lithium hydroxide (0.050 g, 0.00209 mol) and the reaction stirred at room temperature under nitrogen for 2 hours. Then more lithium hydroxide (0.500 g, 0.0209 mol) was added and the reaction stirred at room temperature under nitrogen for 16 hours. The reaction was diluted with ethyl acetate (10.0 mL) and washed with water (10.0 mL). The organic layer was separated, dried with sodium sulphate, filtered and concentrated in vacuo to yield title compound as a pale yellow foam (0.134 g, 0.000374 mol, 99% yield).

後処理

  1. stirringthe reaction stirred at room temperature under nitrogen for 16 hours
  2. washwashed with water (10.0 mL)
  3. customThe organic layer was separated
  4. dry with materialdried with sodium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-6436c74e9df845fcabe15a433073caf9
出典データセット
uspto-grants-2014_04
特許番号
US08685977B2

反応ノート

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