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Methane → HCID 21396807, 화합물

HRID 1439326
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HRID 1439326 반응식
[NH2:1][C:2]([O:9][CH2:10][CH2:11][CH3:12])=[C:3]([C:7]#[N:8])[C:4](=[S:6])[NH2:5].OO.C>C(O)C>[NH2:5][C:4]1[S:6][N:1]=[C:2]([O:9][CH2:10][CH2:11][CH3:12])[C:3]=1[C:7]#[N:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 297MethaneHCID 784Hydrogen PeroxideHCID 85906196HCID 85906196, 화합물

생성물 1

HCID 21396807HCID 21396807, 화합물수율 95.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 111 g of 3-amino-2-cyano-3-propoxypropene-thioamide in 250 ml of ethanol was heated to reflux. To this stirred mixture was added 20.4 g of 30% hydrogen peroxide, at such a rate as to maintain a uniform rate of reflux. After complete addition, the reaction mixture was heated under reflux for 20 minutes. A quantity of activated charcoal was added to the reaction mixture. The reaction mixture was filtered hot and allowed to cool. The filtrate was poured into 1500 ml of water, and the solid precipitate was collected by filtration. The dried solid was recrystallized from toluene, to give 104.5 g of 5-amino-4-cyano-3-propoxyisothiazole, m.p. 122°-125°.

후처리

  1. temperaturewas heated to reflux
  2. temperatureat such a rate as to maintain a uniform rate
  3. temperatureof reflux
  4. additionAfter complete addition
  5. temperaturethe reaction mixture was heated
  6. temperatureunder reflux for 20 minutes
  7. filtrationThe reaction mixture was filtered hot
  8. temperatureto cool
  9. additionThe filtrate was poured into 1500 ml of water
  10. filtrationthe solid precipitate was collected by filtration
  11. customThe dried solid was recrystallized from toluene

출처 및 근거

ORD 기록
ord-45ae10aa13c442d1978445655465de9c
출처 데이터셋
uspto-grants-1977_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04059433

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