Lithium Hydroxide → HCID 66893063, 화합물

HRID 19267노트

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HRID 19267 반응식
C[O:2][C:3](=[O:26])[C@@H:4]([N:12]1[CH2:16][C:15]([O:17][C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([Cl:24])[CH:19]=2)=[CH:14][C:13]1=[O:25])[CH2:5][CH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1.[OH-].[Li+]>O1CCCC1.O>[Cl:24][C:20]1[CH:19]=[C:18]([CH:23]=[CH:22][CH:21]=1)[O:17][C:15]1[CH2:16][N:12]([C@@H:4]([CH2:5][CH:6]2[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]2)[C:3]([OH:26])=[O:2])[C:13](=[O:25])[CH:14]=1

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 66894516(S)-2-[4-(3-chloro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-3-cyclohexyl-propionic acid methyl ester

생성물 1

HCID 66893063HCID 66893063, 화합물수율 86%

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)-2-[4-(3-chloro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-3-cyclohexyl-propionic acid methyl ester (340 mg, 0.9 mmol) in tetrahydrofuran-water (3:1, 10 mL) was added lithium hydroxide (118 mg, 2.7 mmol). 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)-2-[4-(3-chloro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-3-cyclohexyl-propionic acid (280 mg, 86%) 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-bf470c71001d4023b15de42f30ce4a1d
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741327B2

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