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Sodium Hydroxide → HCID 66953683, 화합물

HRID 2096984
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HRID 2096984 반응식
[CH:1]1([NH:4][C:5]([NH:7][NH:8][C:9]2[C:14]([I:15])=[CH:13][CH:12]=[CH:11][N:10]=2)=O)[CH2:3][CH2:2]1.P(Cl)(Cl)(Cl)=O.[OH-].[Na+]>>[CH:1]1([NH:4][C:5]2[N:10]3[CH:11]=[CH:12][CH:13]=[C:14]([I:15])[C:9]3=[N:8][N:7]=2)[CH2:3][CH2:2]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 66954038HCID 66954038, 화합물

생성물 1

HCID 66953683HCID 66953683, 화합물수율 92.6%

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온도
75 °C

실험 절차

A mixture of N-cyclopropyl-2-(3-iodopyridin-2-yl)hydrazinecarboxamide (preparation 26c, 0.56 g, 1.8 mmol) and phosphorous oxychloride (7 mL) was stirred at 75° C. overnight. The reaction mixture was cooled to ambient temperature, added slowly to an ice-water mixture and then was basified to pH 8 with aqueous sodium hydroxide solution. The aqueous solution was extracted with ethyl acetate and the organic layer was washed with brine, dried (MgSO4) and the solvent evaporated in vacuo to yield the title compound (0.50 g, 88%) as a solid.

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후처리

  1. temperatureThe reaction mixture was cooled to ambient temperature
  2. extractionThe aqueous solution was extracted with ethyl acetate
  3. washthe organic layer was washed with brine
  4. dry with materialdried (MgSO4)
  5. customthe solvent evaporated in vacuo

출처 및 근거

ORD 기록
ord-19b793305f8c4aa78f1be84d0a8b11ef
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08450341B2

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