Formaldehyde → 4-oxo-4H-3,1-benzoxazine-8-carboxylic acid

HRID 1842856ノート

反応式

HRID 1842856 の反応式
[NH2:1][C:2]1[C:10]([C:11]([OH:13])=[O:12])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[CH2:14]=O>>[O:5]=[C:4]1[C:3]2[CH:7]=[CH:8][CH:9]=[C:10]([C:11]([OH:13])=[O:12])[C:2]=2[N:1]=[CH:14][O:6]1

参加物

3

反応物 2

HCID 712FormaldehydeHCID 2929162-Aminoisophthalic acid

生成物 1

HCID 676086644-oxo-4H-3,1-benzoxazine-8-carboxylic acid収率 89%

反応条件

温度
140 °C

実験手順

2-Aminoisophthalic acid moiety (50.0 g; 276.0 mmol) and formaldehyde (250.0 ml; 5.00 V) were combined and heated to 140° C. for 4 h. The reaction mixture was cooled to room temperature and distilled under high vacuum on the rotary evaporator. The remaining formaldehyde was removed by azeotropic distillation with toluene. The residue was slurried with ethyl ether, filtered, and the solid was dried under vacuum to provide the desired intermediate (50.3 g, 89% yield).

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. distillationdistilled under high vacuum on the rotary evaporator
  3. customThe remaining formaldehyde was removed by azeotropic distillation with toluene
  4. filtrationfiltered
  5. customthe solid was dried under vacuum

出典と根拠

ORDレコード
ord-aa8514ff7c944df383ff18272029e126
出典データセット
uspto-grants-2015_02
特許番号
US08946247B2

反応ノート

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