Lithium Hydroxide → [4-(4'-Trifluoromethylbiphenyl-2-carbonyl-amino)piperidin-1-yl]acetic acid

HRID 1864969노트

반응식

HRID 1864969 반응식
C([O:3][C:4](=[O:31])[CH2:5][N:6]1[CH2:11][CH2:10][CH:9]([NH:12][C:13]([C:15]2[C:16]([C:21]3[CH:26]=[CH:25][C:24]([C:27]([F:30])([F:29])[F:28])=[CH:23][CH:22]=3)=[CH:17][CH:18]=[CH:19][CH:20]=2)=[O:14])[CH2:8][CH2:7]1)C.[OH-].[Li+]>O1CCCC1CO>[F:30][C:27]([F:28])([F:29])[C:24]1[CH:25]=[CH:26][C:21]([C:16]2[C:15]([C:13]([NH:12][CH:9]3[CH2:8][CH2:7][N:6]([CH2:5][C:4]([OH:31])=[O:3])[CH2:11][CH2:10]3)=[O:14])=[CH:20][CH:19]=[CH:18][CH:17]=2)=[CH:22][CH:23]=1

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 57683250[4-(4'-Trifluoromethylbiphenyl-2-carbonylamino)piperidin-1-yl]acetic acid ethyl ester

생성물 1

HCID 23033209[4-(4'-Trifluoromethylbiphenyl-2-carbonyl-amino)piperidin-1-yl]acetic acid수율 73.8%

시약·촉매·용매 1

HCID 7360Tetrahydrofurfuryl alcohol용매

실험 절차

To a solution of [4-(4′-trifluoromethylbiphenyl-2-carbonylamino)piperidin-1-yl]acetic acid ethyl ester (595 mg) obtained in Example 8c) in tetrahydrofuran-methanol (1:2; 10.2 mL) was added 1M aqueous lithium hydroxide (6.8 mL), and the mixture was stirred at room temperature for 6 hours. The reaction solution was concentrated in vacuo and 2N hydrochloric acid was added to the residue to adjust the pH to about 3, thereby crystals were precipitated. The crystals were collected by filtration, washed with cold water and dried in vacuo to give the title compound (411 mg).

후처리

  1. concentrationThe reaction solution was concentrated in vacuo and 2N hydrochloric acid
  2. additionwas added to the residue
  3. customcrystals were precipitated
  4. filtrationThe crystals were collected by filtration
  5. washwashed with cold water
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-30674e0652fd4d258c243f1008aa8812
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07625948B2

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