Ethanol → HCID 86664945、化合物

HRID 1968929ノート

反応式

HRID 1968929 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-])=O)=[CH:4][C:3]=1[NH:11][C:12](=[O:21])[CH:13]=[CH:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][N:16]=1.C(O)C.[Cl-].[NH4+].C(=O)([O-])[O-].[K+].[K+]>[Fe].O>[NH2:8][C:5]1[CH:6]=[CH:7][C:2]([CH3:1])=[C:3]([NH:11][C:12](=[O:21])/[CH:13]=[CH:14]/[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][N:16]=2)[CH:4]=1

参加物

7

反応物 4

HCID 702EthanolHCID 11430Potassium CarbonateHCID 25517Ammonium ChlorideHCID 67494338HCID 67494338、化合物

生成物 1

HCID 86664945HCID 86664945、化合物

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

8.6 g of the product of step 2 was added to 200 ml ethanol:water (v/v=3/1), then 13.6 g of iron powder and 5.0 g of ammonium chloride were added. After addition, the reaction mixture was heated to 70° C., and reacted for 30 min. The completion of reaction was indicated by TLC. Then the reaction mixture was filtered, washed with hot ethanol repeatedly, and concentrated under reduced pressure to give a yellow solid. 20 ml of potassium carbonate solution (10%) was added to the solid. The mixture was stirred, left to stand, filtered, and dried to give a solid.

後処理

  1. additionAfter addition
  2. customreacted for 30 min
  3. customThe completion of reaction
  4. filtrationThen the reaction mixture was filtered
  5. washwashed with hot ethanol repeatedly
  6. concentrationconcentrated under reduced pressure
  7. customto give a yellow solid
  8. waitleft
  9. filtrationfiltered
  10. customdried
  11. customto give a solid

出典と根拠

ORDレコード
ord-682a942a5ed0444193b4554de5532e60
出典データセット
uspto-grants-2013_04
特許番号
US08426446B2

反応ノート

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