Hydrochloric Acid → HCID 25052183、化合物

HRID 73353ノート

反応式

HRID 73353 の反応式
C([O:3][C:4](=[O:25])[C:5]1[CH:10]=[CH:9][C:8]([N:11]2[C:19]3[C:14](=[CH:15][C:16]([F:21])=[C:17]([F:20])[CH:18]=3)[C:13]([C:22]#[N:23])=[CH:12]2)=[CH:7][C:6]=1[OH:24])C.O1CCCC1.[OH-].[Li+].Cl>O.C(O)C>[C:22]([C:13]1[C:14]2[C:19](=[CH:18][C:17]([F:20])=[C:16]([F:21])[CH:15]=2)[N:11]([C:8]2[CH:9]=[CH:10][C:5]([C:4]([OH:25])=[O:3])=[C:6]([OH:24])[CH:7]=2)[CH:12]=1)#[N:23]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 584372264-(3-Cyano-5,6-difluoroindol-1-yl)-2-hydroxybenzoic acid ethyl ester

生成物 1

HCID 25052183HCID 25052183、化合物収率 88.3%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a solution of 4-(3-cyano-5,6-difluoroindol-1-yl)-2-hydroxybenzoic acid ethyl ester (0.074 g) in a mixed solvent of tetrahydrofuran (3.0 mL) and ethanol (0.75 mL) were added 0.1 g/mL aqueous lithium hydroxide solution (0.62 mL) and water (1.0 mL), and this mixture was stirred at room temperature for 26 hours. To this reaction mixture was added 2 mol/L hydrochloric acid (5 mL), this organic solvent was removed under reduced pressure. This resulting mixture was extracted with ethyl acetate, this organic layer was washed with water, and dried over anhydrous magnesium sulfate. The solvent was concentrated under reduced pressure to give the title compounds (0.06 g).

後処理

  1. customthis organic solvent was removed under reduced pressure
  2. extractionThis resulting mixture was extracted with ethyl acetate
  3. washthis organic layer was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationThe solvent was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-1d0a9a6a73dc4aa487b5054ebe568ad1
出典データセット
uspto-grants-2014_09
特許番号
US08829040B2

反応ノート

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