Hydrogen Bromide → 4,5-Dihydroxy-2-nitrobenzaldehyde

HRID 1982218

反応式

HRID 1982218 の反応式
ClC[O:3][C:4]1[C:5]([OH:15])=[CH:6][C:7]([N+:12]([O-:14])=[O:13])=[C:8]([CH:11]=1)[CH:9]=[O:10].Br>>[OH:15][C:5]1[C:4]([OH:3])=[CH:11][C:8]([CH:9]=[O:10])=[C:7]([N+:12]([O-:14])=[O:13])[CH:6]=1

参加物

3

反応物 2

HCID 260Hydrogen BromideHCID 114247525-Chloromethoxy-4-hydroxy-2-nitrobenzaldehyde

生成物 1

HCID 37823444,5-Dihydroxy-2-nitrobenzaldehyde収率 93%

実験手順

5-Chloromethoxy-4-hydroxy-2-nitrobenzaldehyde (10) (3 g; 0.013 mol) is stirred at 23° C. with 15 ml 48% HBr for two days. The precipitate is removed by filtration, and washed well with H2O, giving 2.2 g (93%) of 4,5-dihydroxy-2-nitrobenzaldehyde (1). The remainder of the product is isolated by ether extraction of the filtrate. Drying the combined ether extracts over Na2SO4, filtering, and removing the ether at reduced pressure, gives the remaining 0.17 g (7%) of (1): mp 201°-203° C.; mass spectrum, m/e 183 (M+); 1HNMR (d6 -Me2CO) δ10.59 (br s,2H), δ10.2(s,1H), δ7.6(s,1H), δ7.3(s,1H).

後処理

  1. customThe precipitate is removed by filtration
  2. washwashed well with H2O

出典と根拠

ORDレコード
ord-152d51ab762c4de391e6b7d9effed8ea
出典データセット
uspto-grants-1986_06
特許番号
US04595765

関連ノート

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