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Pyridine → HCID 19438397、化合物

HRID 374570
ノート
印刷プレビュー

反応式

HRID 374570 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 19438397HCID 19438397、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
40 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-cde20ef7a57f4228aeb7ead0eb08fc11
出典データセット
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05480993

反応ノート

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