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Methanesulfonic Acid → HCID 19812354, 화합물

HRID 373315
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HRID 373315 반응식
[C:1]([C:3]1[C:4]([N:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)=[N:5][CH:6]=[C:7]([C:9]2[CH:14]=[CH:13][N+:12]([O-:15])=[CH:11][CH:10]=2)[CH:8]=1)#[N:2].[CH3:22][S:23]([OH:26])(=[O:25])=[O:24]>CC(C)=O>[CH3:22][S:23]([OH:26])(=[O:25])=[O:24].[C:1]([C:3]1[C:4]([N:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)=[N:5][CH:6]=[C:7]([C:9]2[CH:10]=[CH:11][N+:12]([O-:15])=[CH:13][CH:14]=2)[CH:8]=1)#[N:2]
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참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 10401503HCID 10401503, 화합물

생성물 1

HCID 19812354HCID 19812354, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

0.3 g 3-Cyano-2-morpholino-5,4'-bipyridine-1'-oxide is dissolved in acetone with heating. The solution is allowed to cool, then treated with 0.1 ml methanesulfonic acid and concentrated under vacuum in the rotary evaporator. The oily residue is dissolved in acetone. The resulting solution is mixed with ether until crystallization, then is cooled and filtered with suction. The material filtered out is washed with acetone and ether and dried. Yield: 0.3 g (74.0% of the theoretical yield), the melting point is 151° C.-154° C.

후처리

  1. temperaturewith heating
  2. temperatureto cool
  3. concentrationconcentrated under vacuum in the rotary evaporator
  4. dissolutionThe oily residue is dissolved in acetone
  5. additionThe resulting solution is mixed with ether until crystallization
  6. temperatureis cooled
  7. filtrationfiltered with suction
  8. filtrationThe material filtered out
  9. washis washed with acetone and ether
  10. customdried
  11. customYield: 0.3 g (74.0% of the theoretical yield), the melting point is 151° C.-154° C.

출처 및 근거

ORD 기록
ord-e829f607340f4e09b0156ea115afbc8f
출처 데이터셋
uspto-grants-1992_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05162533

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