Potassium Carbonate → Methyl 3-(cyclopropylmethoxy)-4-nitrobenzoate

HRID 2172582ノート

反応式

HRID 2172582 の反応式
[CH3:1][O:2][C:3](=[O:14])[C:4]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[C:6]([OH:13])[CH:5]=1.C([O-])([O-])=O.[K+].[K+].[CH:21]1([CH2:24]Br)[CH2:23][CH2:22]1>CN(C=O)C.O>[CH3:1][O:2][C:3](=[O:14])[C:4]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[C:6]([O:13][CH2:24][CH:21]2[CH2:23][CH2:22]2)[CH:5]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 81503BromomethylcyclopropaneHCID 294866Methyl 3-hydroxy-4-nitrobenzoate

生成物 1

HCID 59443763Methyl 3-(cyclopropylmethoxy)-4-nitrobenzoate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

3-Hydroxy-4-nitro-benzoic acid methyl ester (10.5 g) was dissolved in dry DMF (150 ml) under N2 atmosphere. K2CO3 (24.3 g), KI (2.6 g) and cyclopropylmethylbromide (10.3 ml) were added and the mixture was stirred at 50° C. for 6 hours. The reaction mixture was diluted with water (300 ml) and extracted with Et2O (2×200 ml); the combined organic layers were dried over Na2SO4 and the solvent was removed by evaporation to yield 12.7 g of the desired intermediate.

後処理

  1. extractionextracted with Et2O (2×200 ml)
  2. dry with materialthe combined organic layers were dried over Na2SO4
  3. customthe solvent was removed by evaporation

出典と根拠

ORDレコード
ord-16eced57828b4f898202ede9b354dd35
出典データセット
uspto-grants-2015_06
特許番号
US09056176B2

反応ノート

読み込み中…