Nitric Acid → 5-Methoxy-4-(3-morpholinopropoxy)-2-nitrobenzoic acid trifluoroacetate

HRID 1597210ノート

反応式

HRID 1597210 の反応式
[N+:1]([O-:4])(O)=[O:2].[CH3:5][O:6][C:7]1[CH:8]=[C:9]([CH:13]=[CH:14][C:15]=1[O:16][CH2:17][CH2:18][CH2:19][N:20]1[CH2:25][CH2:24][O:23][CH2:22][CH2:21]1)[C:10]([OH:12])=[O:11].[C:26]([OH:32])([C:28]([F:31])([F:30])[F:29])=[O:27]>>[F:29][C:28]([F:31])([F:30])[C:26]([OH:32])=[O:27].[CH3:5][O:6][C:7]1[C:15]([O:16][CH2:17][CH2:18][CH2:19][N:20]2[CH2:21][CH2:22][O:23][CH2:24][CH2:25]2)=[CH:14][C:13]([N+:1]([O-:4])=[O:2])=[C:9]([CH:8]=1)[C:10]([OH:12])=[O:11]

参加物

4

反応物 3

HCID 944Nitric AcidHCID 6422Trifluoroacetic acidHCID 216992843-Methoxy-4-(3-morpholinopropoxy)benzoic acid

生成物 1

HCID 694655255-Methoxy-4-(3-morpholinopropoxy)-2-nitrobenzoic acid trifluoroacetate

実験手順

Fuming nitric acid (1.5 ml, 36.2 mmol) was added slowly at 0° C. to a solution of 3-methoxy-4-(3-morpholinopropoxy)benzoic acid (7.78 g, 23.5 mmol) in TFA (25 ml). The cooling bath was removed and the reaction mixture stirred at ambient temperature for 1 hour. The TFA was evaporated and ice was added to the residue. The precipitate was collected by filtration and washed with a minimum of water followed by toluene and ether. The solid was dried under vacuum over phosphorus pentoxide to give 5-methoxy-4-(3-morpholinopropoxy)-2-nitrobenzoic acid trifluoroacetate (7.54 g, 71%yield) which was used without further purification.

後処理

  1. customThe cooling bath was removed
  2. customThe TFA was evaporated
  3. additionice was added to the residue
  4. filtrationThe precipitate was collected by filtration
  5. washwashed with a minimum of water
  6. dry with materialThe solid was dried under vacuum over phosphorus pentoxide

出典と根拠

ORDレコード
ord-da5c8e1c14474ac6bd6156bfbbdeb9ff
出典データセット
uspto-grants-2001_09
特許番号
US06294532B1

反応ノート

読み込み中…