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Water → HCID 20344105, 화합물

HRID 2049639
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HRID 2049639 반응식
[NH2:1][C:2]1[C:11]([N+:12]([O-])=O)=[CH:10][C:9]2[C:4](=[CH:5][C:6]([S:15]([CH2:17][CH:18]([CH3:20])[CH3:19])=[O:16])=[CH:7][CH:8]=2)[CH:3]=1.S(S([O-])=O)([O-])=O.[Na+].[Na+].O>C(O)C>[CH2:17]([S: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)=[O:16])[CH:18]([CH3:20])[CH3:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 24489Sodium DithioniteHCID 20344104HCID 20344104, 화합물

생성물 1

HCID 20344105HCID 20344105, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To 0.025 mole of the 2-amino-7-isobutylsulfinyl-3-nitronaphthalene 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 refluxing 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 10.

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 refluxing 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-90dcfe9befb94babaacb1f621d906f3e
출처 데이터셋
uspto-grants-1980_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04198422

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