Lithium Hydroxide → 2-(3,3-Bis(4-fluorophenyl)-2-oxopiperidin-1-yl)acetic acid

HRID 2408845

반응식

HRID 2408845 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([C:21]3[CH:26]=[CH:25][C:24]([F:27])=[CH:23][CH:22]=3)[CH2:13][CH2:12][CH2:11][N:10]([CH2:14][C:15]([O:17]CC)=[O:16])[C:9]2=[O:20])=[CH:4][CH:3]=1.[OH-].[Li+]>C(O)C.O>[F:27][C:24]1[CH:23]=[CH:22][C:21]([C:8]2([C:5]3[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=3)[CH2:13][CH2:12][CH2:11][N:10]([CH2:14][C:15]([OH:17])=[O:16])[C:9]2=[O:20])=[CH:26][CH:25]=1

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 67359841Ethyl 2-(3,3-bis(4-fluorophenyl)-2-oxopiperidin-1-yl)acetate

생성물 1

HCID 673591112-(3,3-Bis(4-fluorophenyl)-2-oxopiperidin-1-yl)acetic acid

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

The product from Example 23C (0.40 g, 1.07 mmol) was dissolved in ethanol (20 mL). A solution of lithium hydroxide (0.21 g, 8.57 mmol) in water (5 mL) was added and the reaction was heated to 80° C. for 2 hours. The reaction mixture was cooled to room temperature, concentrated, neutralized with 2 N HCl, and then diluted with ethyl acetate. The organic layer was washed with water and brine, dried over magnesium sulfate, filtered, and then concentrated to give the title compound. MS (DCI) m/z 346 (M+H)+.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. concentrationconcentrated
  3. additiondiluted with ethyl acetate
  4. washThe organic layer was washed with water and brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-0a758e08c99c48d68114fbce1d1d197d
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08815869B2

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