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Lithium Hydroxide → 1-(Carboxymethyl)-7-(1-pyrrolyl)-6-trifluoromethyl-2,3(1H,4H)-quinoxalinedione

HRID 861482
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HRID 861482 반응식
C[O:2][C:3]([CH2:5][N:6]1[C:15]2[C:10](=[CH:11][C:12]([C:21]([F:24])([F:23])[F:22])=[C:13]([N:16]3[CH:20]=[CH:19][CH:18]=[CH:17]3)[CH:14]=2)[NH:9][C:8](=[O:25])[C:7]1=[O:26])=[O:4].[OH-].[Li+]>O1CCCC1.O>[C:3]([CH2:5][N:6]1[C:15]2[C:10](=[CH:11][C:12]([C:21]([F:24])([F:23])[F:22])=[C:13]([N:16]3[CH:20]=[CH:19][CH:18]=[CH:17]3)[CH:14]=2)[NH:9][C:8](=[O:25])[C:7]1=[O:26])([OH:4])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 220970571-(Methoxycarbonylmethyl)-7-(1-pyrrolyl)-6-trifluoromethyl-2,3(1H,4H)-quinoxalinedione

생성물 1

HCID 102474741-(Carboxymethyl)-7-(1-pyrrolyl)-6-trifluoromethyl-2,3(1H,4H)-quinoxalinedione수율 69%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

2 g (5.45 mmol) of 1-(methoxycarbonylmethyl)-7-(1-pyrrolyl)-6-trifluoromethyl-2,3(1H,4H)-quinoxalinedione (Example 24) were dissolved in 30 ml of tetrahydrofuran, and 0.4 g (16.4 mmol) of lithium hydroxide dissolved in 4 ml of water was added. The mixture was stirred at room temperature for 16 h and then organic solvent was removed under reduced pressure. The aqueous phase was acidified with 1M hydrochloric acid and extracted with ethyl acetate. The organic phase was dried and concentrated under reduced pressure. The residue was recrystallized from methanol, resulting in 1.3 g (69%) of the product. Melting point 161°-163° C. (decomposition).

후처리

  1. additionwas added
  2. customorganic solvent was removed under reduced pressure
  3. extractionextracted with ethyl acetate
  4. customThe organic phase was dried
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was recrystallized from methanol

출처 및 근거

ORD 기록
ord-f42b68a4b7d74f7c91e4090586998089
출처 데이터셋
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05714489

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