Water → HCID 12888773、化合物

HRID 1719678ノート

反応式

HRID 1719678 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 12888773HCID 12888773、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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. Crystallization from ethanol-ethyl acetate afforded the product m.p. 205° C.

後処理

  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. customCrystallization from ethanol-ethyl acetate

出典と根拠

ORDレコード
ord-a8943e9619eb4dac9a83c23df93db7d8
出典データセット
uspto-grants-1985_09
特許番号
US04542131

反応ノート

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