Water → HCID 20549247, 화합물

HRID 2049635노트

반응식

HRID 2049635 반응식
[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

참가 물질

5

반응물 3

HCID 962WaterHCID 24489Sodium DithioniteHCID 20344111HCID 20344111, 화합물

생성물 1

HCID 20549247HCID 20549247, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ef1067e1a4d145fbb19bbba546b46535
출처 데이터셋
uspto-grants-1980_04
특허 번호
US04198422

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