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HCID 86614660、化合物 → HCID 57713313、化合物

HRID 1983863
ノート
印刷プレビュー

反応式

HRID 1983863 の反応式
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([C:29]3[CH:30]=[C:31](OC(=O)C=C)[CH:32]=[CH:33][CH:34]=3)=[C:7]([CH2:13][C:14]([NH:16][C:17]3[C:22]([C:23]([F:26])([F:25])[F:24])=[CH:21][C:20]([F:27])=[CH:19][C:18]=3[OH:28])=[O:15])[C:8](=[O:12])[O:9]2)=[CH:4][C:3]=1[CH3:40]>C1COCC1.C(O)C.[OH-].[Na+]>[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([C:29]3[CH:30]=[C:31](/[CH:6]=[CH:7]/[C:8]([OH:12])=[O:9])[CH:32]=[CH:33][CH:34]=3)=[C:7]([CH2:13][C:14]([NH:16][C:17]3[C:22]([C:23]([F:26])([F:24])[F:25])=[CH:21][C:20]([F:27])=[CH:19][C:18]=3[OH:28])=[O:15])[C:8](=[O:12])[O:9]2)=[CH:4][C:3]=1[CH3:40]
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 1

HCID 86614660HCID 86614660、化合物

生成物 1

HCID 57713313HCID 57713313、化合物収率 52%

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

Ethyl (2E)-3-{(3-[7-chloro-3-(2-{[4-fluoro-2-hydroxy-6-(trifluoromethyl)phenyl]amino}-2-oxoethyl)-6-methyl-2-oxo-2H-chromen-4-yl]phenyl}acrylate obtained in Reference Example 22 (0.31 g) was dissolved in a mixture of THF (5 ml) and ethanol (5 ml), and 2N aqueous sodium hydroxide solution (1.5 ml) was added thereto. After stirring for 5 hours, the reaction mixture was concentrated. To the residue was added 1N hydrochloric acid and the mixture was extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulfate and concentrated to obtain the title compound as crystals (0.155 g, 52%).

後処理

  1. additionwas added
  2. concentrationthe reaction mixture was concentrated
  3. additionTo the residue was added 1N hydrochloric acid
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe extract was washed with water
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-e2a69905497a49bb86b7a3085b5dd0f8
出典データセット
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07541478B2

反応ノート

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