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Hydrochloric Acid → 6-Diphenylphosphorylamino nicotinamide

HRID 127944
ノート
印刷プレビュー

反応式

HRID 127944 の反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[O:7])=[CH:4][N:3]=1.N1C=CC=CC=1.[C:17]1([P:23](Cl)([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[O:24])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.Cl>N1CCCC1=O.C(O)C.C(Cl)(Cl)Cl>[C:17]1([P:23]([NH:1][C:2]2[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[O:7])=[CH:4][N:3]=2)([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[O:24])[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric Acid2 回HCID 1049PyridineHCID 95006-AminonicotinamideHCID 73910Diphenylphosphinic chloride

生成物 1

HCID 234709116-Diphenylphosphorylamino nicotinamide

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒
HCID 6212
Chloroform
溶媒
HCID 120252-Pyrrolidone溶媒

実験手順

6-Aminonicotinamide 1.37 g (0.01 mole) is dissolved in 10 ml of 2-pyrrolidinone and 3 ml of pyridine by gentle warming of the mixture. Diphenylphosphoryl chloride 6 ml (0.024 mole) is then slowly added to the mixture. After 1 hour of reaction at room temperature, the mixture is poured into 300 ml of 0.2 N HCl. A reddish syrup, 2.2 g which is formed in the bottom of the flask is isolated by decantation. The product may be purified as follows. The reddish syrup obtained above is dissolved in 3 ml of ethanol and the solution is admixed with 200 ml of 0.2 N HCl. Chloroform, 100 ml is added to the mixture to extract the product. After dried over anhydrous sodium sulfate the chloroform solution which contains the product is evaporated at 35° C. in vacuum to give a practically pure 6-diphenylphosphorylamino nicotinamide.

後処理

  1. customAfter 1 hour of reaction at room temperature
  2. customA reddish syrup, 2.2 g which is formed in the bottom of the flask
  3. customis isolated by decantation
  4. customThe product may be purified
  5. customThe reddish syrup obtained
  6. extractionto extract the product
  7. dry with materialAfter dried over anhydrous sodium sulfate the chloroform solution which
  8. customis evaporated at 35° C. in vacuum

出典と根拠

ORDレコード
ord-1d85b24c53974f18bd577b30b6e9f217
出典データセット
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04258052

反応ノート

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