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Sodium Hydroxide → 1-N-(propan-2-yl)benzene-1,2-diamine

HRID 500640
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HRID 500640 반응식
[OH-].[Na+].[CH:3]([NH:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[N+:13]([O-])=O)([CH3:5])[CH3:4]>C(O)C.[Zn]>[NH2:13][C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=1[NH:6][CH:3]([CH3:5])[CH3:4]
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참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 10583518N-Isopropyl-2-nitroaniline

생성물 1

HCID 105587871-N-(propan-2-yl)benzene-1,2-diamine수율 96.3%

시약·촉매·용매 2

HCID 23994Zinc촉매2회HCID 702Ethanol용매2회

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온도
0 °C

실험 절차

To a mixture of ethanol (600 mL) and 2 M sodium hydroxide solution (320 mL) cooled in an ice bath was added Zn dust (59.5 g) slowly. While stirring the Zn slurry, N-isopropyl-N-(2-nitrophenyl)amine (41 g, 0.228 mol) dissolved in ethanol (50 mL) was added. The mixture was stirred at 0° C. for 30 min, then heated to 85° C. The mixture was stirred at 85° C. for about 12 h until the refluxing solution of the mixture became a colorless solution. The mixture was then cooled to 0° C. and filtered. The collected solid was rinsed with ethyl acetate (200 mL). The filtrate and rinsed solution were combined, and evaporated in vacuo to remove excess volatile solvents. During the concentration, the mixture became pale brown/yellow. The aqueous concentrate was extracted with ethyl acetate (800 mL). The organic solution was concentrated to dryness, to provide the title intermediate (33 g) as a brown-pink oil which was used in the next step without further treatment. 1H-NMR (CDCl3, 300 MHz): 6 (ppm) 6.73-6.5 (m, 4H), 3.58-3.55 (hept, 1H), 1.2 (d, 6H).

후처리

  1. temperaturecooled in an ice bath
  2. additionwas added
  3. temperatureheated to 85° C
  4. stirringThe mixture was stirred at 85° C. for about 12 h until the refluxing solution of the mixture
  5. temperatureThe mixture was then cooled to 0° C.
  6. filtrationfiltered
  7. washThe collected solid was rinsed with ethyl acetate (200 mL)
  8. washThe filtrate and rinsed solution
  9. customevaporated in vacuo
  10. customto remove excess volatile solvents
  11. concentrationDuring the concentration
  12. concentrationThe aqueous concentrate
  13. extractionwas extracted with ethyl acetate (800 mL)
  14. concentrationThe organic solution was concentrated to dryness

출처 및 근거

ORD 기록
ord-5d0109f158a944fcb0b2f0b87399e240
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07772239B2

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