Methanol → HCID 178481705, 화합물

HRID 444555

반응식

HRID 444555 반응식
[C:1]([NH:5][NH2:6])(=O)[CH2:2][OH:3].[CH3:7][N:8]=[C:9]=[S:10].CO.[Na]>C(O)C>[OH:3][CH2:2][C:1]1[N:8]([CH3:7])[C:9]([SH:10])=[N:6][N:5]=1

참가 물질

6

반응물 4

HCID 887MethanolHCID 11167Methyl isothiocyanateHCID 3505362-HydroxyacetohydrazideHCID 5360545Sodium

생성물 1

HCID 178481705HCID 178481705, 화합물수율 35.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 9 g of glycolic acid hydrazide, 7.3 g of methyl isothiocyanate, 50 ml of methanol and 50 ml of ethanol was heated under reflux for 5 hours. Following the addition of 2.3 g of sodium metal, the mixture was further refluxed for 24 hours. The reaction mixture was concentrated under reduced pressure and the residue was dissolved in 150 ml of water and adjusted to pH 2.5 with phosphoric acid. The resultant crystals were collected by filtration and recrystallized from ethanol. By the above procedure there were obtained 5.2 g of the captioned compound. m.p. 199°-201° C.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 5 hours
  3. temperaturethe mixture was further refluxed for 24 hours
  4. concentrationThe reaction mixture was concentrated under reduced pressure
  5. dissolutionthe residue was dissolved in 150 ml of water
  6. filtrationThe resultant crystals were collected by filtration
  7. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-2a9cfc64dc5e44e7a2c3edc3180ea0a0
출처 데이터셋
uspto-grants-1981_04
특허 번호
US04264595

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