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Lithium Hydroxide → HCID 66894715, 화합물

HRID 19253
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HRID 19253 반응식
C[O:2][C:3](=[O:27])[C@@H:4]([N:12]1[CH2:16][C:15]([O:17][C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[C:19]=2[CH3:25])=[CH:14][C:13]1=[O:26])[CH2:5][CH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1.[OH-].[Li+]>O1CCCC1.O>[CH:6]1([CH2:5][C@H:4]([N:12]2[CH2:16][C:15]([O:17][C:18]3[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[C:19]=3[CH3:25])=[CH:14][C:13]2=[O:26])[C:3]([OH:27])=[O:2])[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1
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참가 물질

4

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HCID 3939Lithium HydroxideHCID 66894490(S)-3-cyclohexyl-2-[4-(2,3-dimethyl-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-propionic acid methyl ester

생성물 1

HCID 66894715HCID 66894715, 화합물수율 100.7%

시약·촉매·용매 1

HCID 21881883Oxolane--water (1/1)용매

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온도
23 °C

실험 절차

To a stirred solution of (S)-3-cyclohexyl-2-[4-(2,3-dimethyl-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-propionic acid methyl ester (850 mg, 0.002 mol) in tetrahydrofuran-water (3:1, 10 mL) was added lithium hydroxide (287 mg, 0.012 mol). The reaction mixture was stirred at 23° C. for 2 h. After this time, the mixture was concentrated and the reaction mixture was diluted with water. The reaction mixture was acidified with 2N hydrochloric acid, during which time precipitation occurred. The precipitate was removed by filtration, washed with cold water and dried in vacuo to obtain (S)-3-cyclohexyl-2-[4-(2,3-dimethyl-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-propionic acid (720 mg, 88%) as an off-white solid.

후처리

  1. concentrationAfter this time, the mixture was concentrated
  2. additionthe reaction mixture was diluted with water
  3. customThe reaction mixture was acidified with 2N hydrochloric acid, during which time precipitation
  4. customThe precipitate was removed by filtration
  5. washwashed with cold water
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-d25a97f750f8449cb79c720ec04a1ce9
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07741327B2

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