Water → HCID 20549247、化合物

HRID 2049635ノート

反応式

HRID 2049635 の反応式
[NH2:1][C:2]1[C:11]([N+:12]([O-])=O)=[CH:10][C:9]2[C:4](=[CH:5][C:6]([Cl:15])=[CH:7][CH:8]=2)[CH:3]=1.S(S([O-])=O)([O-])=O.[Na+].[Na+].O>C(O)C>[Cl:15][C:6]1[CH:5]=[C:4]2[C:9]([CH:10]=[C:11]([NH2:12])[C:2]([NH2:1])=[CH:3]2)=[CH:8][CH:7]=1

参加物

5

反応物 3

HCID 962WaterHCID 24489Sodium DithioniteHCID 20344111HCID 20344111、化合物

生成物 1

HCID 20549247HCID 20549247、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To 0.025 mole of the 2-amino-7-chloro-3-nitronaphthalene (prepared in Example 2) in 100 ml of 95% ethanol is added a solution of 3.4 equivalents of sodium hydrosulfite (Na2S2O4) in a solution of 100 ml of water and 15 ml concentrated (28%) ammonium hydroxide. The mixture is refluxed for 5 minutes and an amount of hydrosulfite solution equal to 10% of the original is added to the relfuxing mixture. TLC (silica gel, ether) indicates consumption of starting material. The mixture is concentrated to one-half its original volume under vacuum and the residual mixture extracted with two 150 ml portions of chloroform. The combined chloroform extracts are dried (Na2SO4), filtered, and evaporated to dryness to yield the crude title compound which is used without further purification in Example 4.

後処理

  1. concentrationconcentrated (28%) ammonium hydroxide
  2. temperatureThe mixture is refluxed for 5 minutes
  3. additionan amount of hydrosulfite solution equal to 10% of the original is added to the relfuxing mixture
  4. customconsumption of starting material
  5. concentrationThe mixture is concentrated to one-half its original volume under vacuum
  6. extractionthe residual mixture extracted with two 150 ml portions of chloroform
  7. dry with materialThe combined chloroform extracts are dried (Na2SO4)
  8. filtrationfiltered
  9. customevaporated to dryness

出典と根拠

ORDレコード
ord-ef1067e1a4d145fbb19bbba546b46535
出典データセット
uspto-grants-1980_04
特許番号
US04198422

反応ノート

読み込み中…