Ammonium formate → HCID 70673729、化合物

HRID 341332ノート

反応式

HRID 341332 の反応式
[N+:1]([CH2:4][CH:5]([Si:17]([CH3:20])([CH3:19])[CH3:18])[CH2:6][C:7]([O:9]CC1C=CC=CC=1)=[O:8])([O-])=O.C([O-])=O.[NH4+]>CO.[Pd]>[NH2:1][CH2:4][CH:5]([Si:17]([CH3:18])([CH3:20])[CH3:19])[CH2:6][C:7]([OH:9])=[O:8]

参加物

5

反応物 2

HCID 2723923Ammonium formateHCID 70673606HCID 70673606、化合物

生成物 1

HCID 70673729HCID 70673729、化合物収率 86%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A suspension of benzyl 4-nitro-3-(trimethylsilyl)butanoate (797 mg, 2.70 mmol) and palladium/carbon (10%, 165 mg) in methanol (30 ml) was added with ammonium formate (1.70 g, 27.0 mmol), and the mixture was stirred under an argon atmosphere for 40 hours. The reaction mixture was filtered through Celite, and the Celite layer was washed with methanol. The reaction mixture was concentrated under reduced pressure, and the residue was purified by recrystallization and silica gel chromatography [methanol (10 to 25%)/chloroform] to obtain 4-amino-3-(trimethylsilyl)butanoic acid (406 mg, 86%) mentioned in the title as colorless powder.

後処理

  1. filtrationThe reaction mixture was filtered through Celite
  2. washthe Celite layer was washed with methanol
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. customthe residue was purified by recrystallization and silica gel chromatography [methanol (10 to 25%)/chloroform]

出典と根拠

ORDレコード
ord-4da1b9521dad4bc6b35897948c716102
出典データセット
uspto-grants-2014_11
特許番号
US08895769B2

反応ノート

読み込み中…