Water → HCID 12888773, 화합물

HRID 1995275노트

반응식

HRID 1995275 반응식
[NH2:1][C:2]1[C:6]([C:7]#[N:8])=[CH:5][N:4]([CH3:9])[N:3]=1.[H-].[Na+].Cl[C:13]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=1[N+:20]([O-:22])=[O:21].O>O1CCCC1>[Cl:19][C:16]1[CH:17]=[CH:18][C:13]([NH:1][C:2]2[C:6]([C:7]#[N:8])=[CH:5][N:4]([CH3:9])[N:3]=2)=[C:14]([N+:20]([O-:22])=[O:21])[CH:15]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 69772,5-DichloronitrobenzeneHCID 24758Sodium hydrideHCID 106542131-Methyl-3-amino-4-cyanopyrazole

생성물 1

HCID 12888773HCID 12888773, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

3-Amino-1-methylpyrazole-4-carbonitrile (Helv. Chim. Acta (1959) 42 763) (3.66 g) was stirred in dry tetrahydrofuran (40 ml). Sodium hydride (50% oil dispersion, 2.28 g) was added and the mixture was stirred for 10 minutes. 2,5-Dichloronitrobenzene (5.76 g) was added and the solution stirred under nitrogen for 20 hours. Water was added dropwise to destroy any excess sodium hydride, then the solution was poured on to a mixture of ice and dilute hydrochloric acid. After standing for 1 hour the brick-red precipitate was filtered, washed with water and dried. Crystallisation from ethanol-ethyl acetate afforded the product m.p. 205° C.

후처리

  1. stirringthe solution stirred under nitrogen for 20 hours
  2. customto destroy any excess sodium hydride
  3. additionthe solution was poured on to a mixture of ice and dilute hydrochloric acid
  4. waitAfter standing for 1 hour
  5. filtrationthe brick-red precipitate was filtered
  6. washwashed with water
  7. customdried
  8. customCrystallisation from ethanol-ethyl acetate

출처 및 근거

ORD 기록
ord-8616279523904d728be7509e0859123b
출처 데이터셋
uspto-grants-1983_09
특허 번호
US04404137

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