Nitric Acid → 7-nitro-2,3,4,5-tetrahydro-1H-1-benzazepin-2-one

HRID 518835

反応式

HRID 518835 の反応式
[NH:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[CH2:5][CH2:4][CH2:3][C:2]1=[O:12].[N+:13]([O-])([OH:15])=[O:14].S(=O)(=O)(O)O>O>[N+:13]([C:10]1[CH:9]=[CH:8][C:7]2[NH:1][C:2](=[O:12])[CH2:3][CH2:4][CH2:5][C:6]=2[CH:11]=1)([O-:15])=[O:14]

参加物

5

反応物 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 2485801,3,4,5-Tetrahydro-2H-1-benzazepin-2-one

生成物 1

HCID 3561757-nitro-2,3,4,5-tetrahydro-1H-1-benzazepin-2-one

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
0 °C

実験手順

2 g of 1,3,4,5-tetrahydro-2H-1-benzazepin-2-one are added to a solution of 25 ml of nitric acid at 70% in water and of 35 ml of sulfuric acid cooled to 0° C. The reaction medium is stirred for 15 minutes at 0° C. and then poured into water (250 ml) and extracted with ethyl acetate. The organic phase is washed with a saturated aqueous sodium bicarbonate solution and with water, dried over magnesium sulfate, filtered and concentrated under reduced pressure. The residue is taken up with diisopropyl ether and the insoluble material is filtered off and dried under vacuum, so as to give 1.04 g of 7-nitro-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one in the form of a beige solid.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic phase is washed with a saturated aqueous sodium bicarbonate solution and with water
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. filtrationthe insoluble material is filtered off
  7. customdried under vacuum

出典と根拠

ORDレコード
ord-a220b8ec54d947ea9832a6d3eb76f824
出典データセット
uspto-grants-2015_08
特許番号
US09115140B2

関連ノート

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