Nitric Acid → 7-Nitro-2,3-dihydro-1,4-benzodioxine-5-carboxylic acid

HRID 127418ノート

反応式

HRID 127418 の反応式
C(OC(=O)C)(=O)C.[O:8]1[C:13]2[CH:14]=[CH:15][CH:16]=[C:17]([C:18]([OH:20])=[O:19])[C:12]=2[O:11][CH2:10][CH2:9]1.[N+:21]([O-])([OH:23])=[O:22]>C(O)(=O)C>[N+:21]([C:15]1[CH:16]=[C:17]([C:18]([OH:20])=[O:19])[C:12]2[O:11][CH2:10][CH2:9][O:8][C:13]=2[CH:14]=1)([O-:23])=[O:22]

参加物

5

反応物 3

HCID 944Nitric AcidHCID 7918Acetic AnhydrideHCID 781842,3-Dihydro-1,4-benzodioxin-5-carboxylic acid

生成物 1

HCID 124645337-Nitro-2,3-dihydro-1,4-benzodioxine-5-carboxylic acid収率 27%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

160 ml of acetic acid, 160 ml of acetic anhydride and 100 g of 1,4-benzodioxane-5-carboxylic acid were introduced into a balloon flask provided with an agitator and a thermometer. The mixture was heated and a solution of 40 ml of nitric acid in 40 ml of acetic acid was added. The mixture was agitated at 40°-45° C. and then cooled. The crystals were dried off, washed and dried. 34 g of 7-nitro-1,4-benzodioxane-5-carboxylic acid were obtained (M.P.: 246° C.; yield: 27%).

後処理

  1. customprovided with an agitator
  2. temperatureThe mixture was heated
  3. temperaturecooled
  4. customThe crystals were dried off
  5. washwashed
  6. customdried

出典と根拠

ORDレコード
ord-434a3bde22194d64ae3866962a44bed1
出典データセット
uspto-grants-1981_03
特許番号
US04255580

反応ノート

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