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Ammonium Hydroxide → 1-ethyl-5-(2-methanesulfonylethyl)-1H-pyrazole-3-carbonitrile

HRID 1360421
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반응식

HRID 1360421 반응식
[CH2:1]([N:3]1[C:7]([CH2:8][CH2:9][S:10]([CH3:13])(=[O:12])=[O:11])=[CH:6][C:5]([C:14]([NH2:16])=O)=[N:4]1)[CH3:2].[OH-].[NH4+]>P(Cl)(Cl)(Cl)=O>[CH2:1]([N:3]1[C:7]([CH2:8][CH2:9][S:10]([CH3:13])(=[O:12])=[O:11])=[CH:6][C:5]([C:14]#[N:16])=[N:4]1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14923Ammonium HydroxideHCID 66958625HCID 66958625, 화합물

생성물 1

HCID 669591691-ethyl-5-(2-methanesulfonylethyl)-1H-pyrazole-3-carbonitrile수율 96.7%

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

실험 절차

A modification of the method described in Part E of Examples 1-4 was used to treat 1-ethyl-5-(2-methanesulfonylethyl)-1H-pyrazole-3-carboxamide (3.46 g, 14.1 mmol) with phosphorous oxychloride (10 mL). The reaction was heated for 2.5 hours. After the addition of ammonium hydroxide (35 mL of 28%) a precipitate formed. The mixture was stirred for 30 minutes, and the precipitate was isolated by filtration and washed with water to provide 3.1 g of 1-ethyl-5-(2-methanesulfonylethyl)-1H-pyrazole-3-carbonitrile as a white powder.

후처리

  1. temperatureThe reaction was heated for 2.5 hours
  2. customformed
  3. customthe precipitate was isolated by filtration
  4. washwashed with water

출처 및 근거

ORD 기록
ord-47c6a6624f97476b98c0014b4e2d3b2d
출처 데이터셋
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07879849B2

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