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Pyridine → HCID 19438397, 화합물

HRID 374570
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HRID 374570 반응식
[O-:1][C:2]#[N:3].[Na+].[N:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[CH2:11]([O:13][C:14]([C:16]1[CH:17]=[N:18][N:19]([CH3:25])[C:20]=1[S:21](Cl)(=[O:23])=[O:22])=[O:15])[CH3:12]>C(#N)C>[OH-:1].[CH2:11]([O:13][C:14]([C:16]1[CH:17]=[N:18][N:19]([CH3:25])[C:20]=1[S:21]([NH:3][C:2]([N+:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:1])(=[O:23])=[O:22])=[O:15])[CH3:12]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 517096Sodium CyanateHCID 10977963ethyl 5-(chlorosulfonyl)-1-methyl-1H-pyrazole-4-carboxylate

생성물 1

HCID 19438397HCID 19438397, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
40 °C

실험 절차

1.08 g (16.6 mmole) of anhydrous sodium cyanate, 1.25 g (15.8 mmole) of dry pyridine and 20.0 g of dry acetonitrile were mixed together and the resulting mixture was then stirred under nitrogen atmosphere while maintaining the temperature of 40° C. To this mixture was added 3.80 g (15.0 mmole) of 4-ethoxycarbonyl-1-methylpyrazole-5-sulfonylchloride over one hour. The reaction mixture was then stirred for further 2 hours while maintaining the temperature of 40° to 45° C. to complete the reaction. After the reaction was completed, the reaction solution was filtered under nitrogen atmosphere. The solvent and the remaining pyridine were removed from the filtrate at normal temperature by means of a vacuum pump to obtain the crude product which was then washed with 10.00 g of dry ethyl ether and dried to obtain 4.68 g (Yieid 92%) of the title compound as the white solid.

후처리

  1. stirringThe reaction mixture was then stirred for further 2 hours
  2. temperaturewhile maintaining the temperature of 40° to 45° C.
  3. customthe reaction
  4. filtrationthe reaction solution was filtered under nitrogen atmosphere
  5. customThe solvent and the remaining pyridine were removed from the filtrate at normal temperature by means of a vacuum pump
  6. customto obtain the crude product which
  7. washwas then washed with 10.00 g of dry ethyl ether
  8. customdried

출처 및 근거

ORD 기록
ord-cde20ef7a57f4228aeb7ead0eb08fc11
출처 데이터셋
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05480993

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