Hydrochloric Acid → 2-[5-chloro-2-[2-(1-naphthyl)propanoylamino]phenylmethyl]Benzoic Acid

HRID 50145ノート

反応式

HRID 50145 の反応式
C[O:2][C:3](=[O:33])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[CH2:10][C:11]1[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:12]=1[NH:18][C:19](=[O:32])[CH:20]([C:22]1[C:31]2[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=2)[CH:25]=[CH:24][CH:23]=1)[CH3:21].[OH-].[Na+].Cl>>[Cl:17][C:15]1[CH:14]=[CH:13][C:12]([NH:18][C:19](=[O:32])[CH:20]([C:22]2[C:31]3[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=3)[CH:25]=[CH:24][CH:23]=2)[CH3:21])=[C:11]([CH2:10][C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[C:3]([OH:33])=[O:2])[CH:16]=1

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 102046962-[5-chloro-2-[2-(1-naphthyl)propanoylamino]phenylmethyl]Benzoic Acid Methyl Ester

生成物 1

HCID 101143682-[5-chloro-2-[2-(1-naphthyl)propanoylamino]phenylmethyl]Benzoic Acid収率 80.2%

反応条件

温度
50 °C

実験手順

To a solution of 2-[5-chloro-2-[2-(1-naphthyl) propanoylamino]phenyl methyl]benzoic acid methyl ester (440 mg; prepared in Example 1.) in methanol-dioxane (1:1; 8 ml) was added 2 mol/L aqueous solution of sodium hydroxide (3 ml) and the mixture was stirred for 3 hours at 50° C. The solution was acidified with hydrochloric acid and was extracted with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride, dried and concentrated to give a crude crystal. It was washed with ethyl acetate-hexane to give the title compound (342 mg; white powder) having the following physical data.

後処理

  1. extractionwas extracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materiala saturated aqueous solution of sodium chloride, dried
  4. concentrationconcentrated
  5. customto give a crude crystal
  6. washIt was washed with ethyl acetate-hexane

出典と根拠

ORDレコード
ord-110c2320b5094ee0958289bc3d81c4b2
出典データセット
uspto-grants-2004_03
特許番号
US06710205B2

反応ノート

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