Diethyl Sulfate → Ethyl 2-amino-6-nitrobenzoate

HRID 231582

反応式

HRID 231582 の反応式
[NH2:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([N+:11]([O-:13])=[O:12])[C:3]=1[C:4]([OH:6])=[O:5].[CH2:14](OS(OCC)(=O)=O)[CH3:15].C(N(CC)CC)C>>[NH2:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([N+:11]([O-:13])=[O:12])[C:3]=1[C:4]([O:6][CH2:14][CH3:15])=[O:5]

参加物

4

反応物 3

HCID 6163Diethyl SulfateHCID 8471TriethylamineHCID 957952-Amino-6-nitro-benzoic acid

生成物 1

HCID 20033751Ethyl 2-amino-6-nitrobenzoate

実験手順

A solution of 2-amino-6-nitrobenzoic acid (29.2 g, 0.16 mol), diethylsulfate (24.7 g, 0.160 mol) and triethylamine (16.2 g, 0.160 mol) in N-dimethylformamide (250 ml) was stirred at 20-25° for 20 hours. After removing DMF at 60° and 0.2 mm pressure, the residue was flash chromotographed over silica gel and the ethyl ester (10.8 g) eluted first with toluene then with 50% toluene-50% chloroform.

後処理

  1. customAfter removing DMF at 60°
  2. washthe ethyl ester (10.8 g) eluted first with toluene

出典と根拠

ORDレコード
ord-c2b21851377d4ef093985a94dcaa0ab0
出典データセット
uspto-grants-1989_07
特許番号
US04847294

関連ノート

読み込み中…