Lithium Hydroxide → [7-(3-Chlorophenyl)-1-oxo-1,2,3,4-tetrahydropyrrolo[1,2-a]pyrazin-4-yl]acetic acid

HRID 711401노트

반응식

HRID 711401 반응식
C([O:3][C:4](=[O:23])[CH2:5][CH:6]1[N:11]2[CH:12]=[C:13]([C:15]3[CH:20]=[CH:19][CH:18]=[C:17]([Cl:21])[CH:16]=3)[CH:14]=[C:10]2[C:9](=[O:22])[NH:8][CH2:7]1)C.[OH-].[Li+]>O1CCCC1.O>[Cl:21][C:17]1[CH:16]=[C:15]([C:13]2[CH:14]=[C:10]3[C:9](=[O:22])[NH:8][CH2:7][CH:6]([CH2:5][C:4]([OH:23])=[O:3])[N:11]3[CH:12]=2)[CH:20]=[CH:19][CH:18]=1

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 86731547Ethyl [7-(3-chlorophenyl)-1-oxo-1,2,3,4-tetrahydropyrrolo[1,2-a]pyrazin-4-yl]acetate

생성물 1

HCID 56766546[7-(3-Chlorophenyl)-1-oxo-1,2,3,4-tetrahydropyrrolo[1,2-a]pyrazin-4-yl]acetic acid수율 85.9%

시약·촉매·용매 1

HCID 21881883Oxolane--water (1/1)용매

실험 절차

To a solution of ethyl[7-(3-chlorophenyl)-1-oxo-1,2,3,4-tetrahydropyrrolo[1,2-a]pyrazin-4-yl]acetate (0.573 g, 1.72 mmol) in a mixture tetrahydrofuran-water (5:1, 10 mL) was added lithium hydroxide (144 mg, 3.44 mmol) and the reaction mixture was stirred at room temperature for 18 h. The THF was evaporated and the aqueous residue diluted with H2O. The aqueous phase was acidified with hydrochloric acid (1 M) until pH<1 and a precipitation occurred; the solid was filtered, washed with water and dried under vacuum to obtain the title compound as an off-white solid (450 mg, 85% yield).

후처리

  1. customThe THF was evaporated
  2. additionthe aqueous residue diluted with H2O
  3. customa precipitation
  4. filtrationthe solid was filtered
  5. washwashed with water
  6. customdried under vacuum

출처 및 근거

ORD 기록
ord-6b14ff4e913a49959971a906dcd407c2
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181258B2

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