Hydrochloric Acid → 2-(2,4-Dinitrophenyl)propane-1,3-diol

HRID 523339

반응식

HRID 523339 반응식
[N+:1]([C:4]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[CH:7]=[CH:6][C:5]=1[CH3:13])([O-:3])=[O:2].[CH2:14]=[O:15].[K].Cl.CN1[C:23](=[O:24])CCC1>>[N+:1]([C:4]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[CH:7]=[CH:6][C:5]=1[CH:13]([CH2:23][OH:24])[CH2:14][OH:15])([O-:3])=[O:2]

참가 물질

6

반응물 5

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 84612,4-DinitrotolueneHCID 13387N-methyl-2-pyrrolidoneHCID 5462222Potassium

생성물 1

HCID 136636452-(2,4-Dinitrophenyl)propane-1,3-diol

실험 절차

20 g (106.5 mmol) of 2,4-dinitrotoluene is solubilized in 280 ml of NMP. To the brown solution is added 7.6 g (255.6 mmol) of paraformaldehyde. To the suspension is added 597 mg (5.32 mmol) of potassium tetrabutoxyde. The resulting solution is stirred overnight at RT. The mixture was poured onto 200 ml ice, and neutralized with 2 mL of HCl 25%. The reaction mixture is then partitioned between ethyl acetate and water; the organic phase is washed repeatedly with water, dried over sodium sulfate, filtered and concentrated by rotary evaporation. The solution is precipitate at RT by adding 150 ml of heptane. The product is filtrated and dried under vacuum at RT to give 16.1 g of 2-(2,4-dinitrophenyl)propane-1,3-diol as a slightly yellow product.

후처리

  1. customThe reaction mixture is then partitioned between ethyl acetate and water
  2. washthe organic phase is washed repeatedly with water
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated by rotary evaporation
  6. customat RT
  7. additionby adding 150 ml of heptane
  8. filtrationThe product is filtrated
  9. customdried under vacuum at RT

출처 및 근거

ORD 기록
ord-ab2ab9de26124aafbeba70c8a8f3eca1
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09334366B2

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