Lithium Hydroxide → HCID 58046316, 화합물

HRID 2359306노트

반응식

HRID 2359306 반응식
[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]

참가 물질

6

반응물 2

HCID 3939Lithium Hydroxide2회HCID 58046348Benzoic acid, 4-[4-chloro-3-(trifluoromethyl)phenoxy]-2-(methoxymethyl)-, methyl ester

생성물 1

HCID 58046316HCID 58046316, 화합물수율 100%

시약·촉매·용매 3

HCID 962Water용매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-6436c74e9df845fcabe15a433073caf9
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08685977B2

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