Urea → N-(2-propylpentanoyl)urea

HRID 83977

반응식

HRID 83977 반응식
[C:1](Cl)(=[O:9])[CH:2]([CH2:6][CH2:7][CH3:8])[CH2:3][CH2:4][CH3:5].S(Cl)(Cl)=O.C(O)(=O)C(CCC)CCC.[NH2:25][C:26]([NH2:28])=[O:27]>C(#N)C>[CH2:3]([CH:2]([CH2:6][CH2:7][CH3:8])[C:1]([NH:25][C:26]([NH2:28])=[O:27])=[O:9])[CH2:4][CH3:5]

참가 물질

6

반응물 4

HCID 1176UreaHCID 3121Valproic AcidHCID 24386Thionyl ChlorideHCID 762402-Propylvaleryl chloride

생성물 1

HCID 80191N-(2-propylpentanoyl)urea

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

Valproyl chloride (0.057 mol), prepared by coupling of thionylchloride and valproic acid according to a published method [24], was dissolved in dry acetonitrile (50 ml), and the resulting solution was slowly added to a boiling solution of urea (0.14 mole) in dry acetonitrile (100 ml) and allowed to reflux for 2 hours. Thereafter the organic solvent was evaporated under reduced pressure and the product was dissolved in ethyl acetate (100 ml) and washed three times with 20 ml of distilled water. The organic fraction was dried over MgSO4, filtered and evaporated under reduced pressure. The products were purified by crystallization from ethyl acetate.

후처리

  1. temperatureto reflux for 2 hours
  2. customThereafter the organic solvent was evaporated under reduced pressure
  3. dissolutionthe product was dissolved in ethyl acetate (100 ml)
  4. washwashed three times with 20 ml of distilled water
  5. dry with materialThe organic fraction was dried over MgSO4
  6. filtrationfiltered
  7. customevaporated under reduced pressure
  8. customThe products were purified by crystallization from ethyl acetate

출처 및 근거

ORD 기록
ord-b43ccd2aa5be4a4bb1e813a1bc026e6d
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846903B2

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