Sodium Bicarbonate → 1-(2-Methoxymethyl-3-bromophenyl)-4-methyl-1,4-dihydrotetrazol-5-one

HRID 628495ノート

反応式

HRID 628495 の反応式
Br[CH2:2][C:3]1[C:8]([Br:9])=[CH:7][CH:6]=[CH:5][C:4]=1[N:10]1[C:14](=[O:15])[N:13]([CH3:16])[N:12]=[N:11]1.C[O-].[Na+].[C:20](=O)(O)[O-:21].[Na+]>O1CCCC1>[CH3:20][O:21][CH2:2][C:3]1[C:8]([Br:9])=[CH:7][CH:6]=[CH:5][C:4]=1[N:10]1[C:14](=[O:15])[N:13]([CH3:16])[N:12]=[N:11]1

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 10942334Sodium MethoxideHCID 898756621-(2-Bromomethyl-3-bromophenyl)-4-methyl-1,4-dihydrotetrazol-5-one

生成物 1

HCID 898762251-(2-Methoxymethyl-3-bromophenyl)-4-methyl-1,4-dihydrotetrazol-5-one

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 1-(2-bromomethyl-3-bromophenyl)-4-methyl-1,4-dihydrotetrazole-5-one 45.0 g, sodium methoxide 37.4 g and tetrahydrofuran 600 ml was stirred at room temperature for three hours. To the reaction mixture was added aqueous saturated sodium bicarbonate solution and the resulting mixture was extracted with ethyl acetate. The organic layer was washed with aqueous saturated sodium bicarbonate solution and was dried over anhydrous magnesium sulfate. The resulting mixture was concentrated under reduced pressure to give 1-(2-methoxymethyl-3-bromophenyl)-4-methyl-1,4-dihydrotetrazole-5-one 36.2 g.

後処理

  1. extractionthe resulting mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with aqueous saturated sodium bicarbonate solution
  3. dry with materialwas dried over anhydrous magnesium sulfate
  4. concentrationThe resulting mixture was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-64e1bc762b704889896dddabedffa327
出典データセット
uspto-grants-2016_04
特許番号
US09314023B2

反応ノート

読み込み中…