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

HRID 861482
ノート
印刷プレビュー

反応式

HRID 861482 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f42b68a4b7d74f7c91e4090586998089
出典データセット
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05714489

反応ノート

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