Hydrochloric Acid → Methyl 4-aminobenzenebutanoate

HRID 916497

反応式

HRID 916497 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][CH2:10][C:11]([OH:13])=[O:12])=[CH:4][CH:3]=1.Cl.[C:15]([O-])(O)=O.[Na+].C([O-])([O-])=O.[Na+].[Na+]>CO>[CH3:15][O:12][C:11](=[O:13])[CH2:10][CH2:9][CH2:8][C:5]1[CH:4]=[CH:3][C:2]([NH2:1])=[CH:7][CH:6]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 270494-(4-Aminophenyl)butanoic acidHCID 516892Sodium Bicarbonate

生成物 1

HCID 88628Methyl 4-aminobenzenebutanoate収率 91%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

To a solution of 4-(4-aminophenyl)-butyric acid (5 g, 27.90 mmol) in MeOH (100 mL) at room temperature was added HCl conc. (37% 15 mL). The resulting mixture was stirred overnight at 50° C. then treated with a saturated aqueous solution NaHCO3 and Na2CO3 solid until pH 9. The solvent was evaporated under reduced pressure then the aqueous phase was extracted several times with CH2Cl2. The crude material was purified by flash chromatography using CH2Cl2/MeOH as solvent mixture yielding 40 (4.93 g, 91%) as orange solid.

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. extractionthe aqueous phase was extracted several times with CH2Cl2
  3. customThe crude material was purified by flash chromatography

出典と根拠

ORDレコード
ord-c8e20f890da04c3e8d60e09bd7268c1d
出典データセット
uspto-grants-2007_09
特許番号
USRE039850E1

関連ノート

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