(4-Chlorophenyl)hydrazine → HCID 178479604、化合物

HRID 649579ノート

反応式

HRID 649579 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][NH2:9])=[CH:4][CH:3]=1.Cl[C:11]1[C:16]([C:17](OCC)=[O:18])=[CH:15][N:14]=[C:13]2[CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][C:12]=12>C(O)CCC>[ClH:1].[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:17](=[O:18])[C:16]3[C:11]([C:12]4[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][C:13]=4[NH:14][CH:15]=3)=[N:9]2)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 70624(4-Chlorophenyl)hydrazineHCID 21270435Ethyl 4-chloro-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridine-3-carboxylate

生成物 1

HCID 178479604HCID 178479604、化合物

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

A mixture of 2.6 g of p-chlorophenylhydrazine and 3.9 g of ethyl 4-chloro-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridine-3-carboxylate (Example 2c) in 100 mL of n-butanol is refluxed overnight under nitrogen atmosphere, then cooled to room temperature. The solid precipitate is collected, triturated with ether, dissolved in hot ethanol and decolorized with charcoal. The ethanolic solution is acidified with hydrogen chloride, then concentrated to a smaller volume and diluted with ether to precipitate a yellow solid, which is collected, washed with ether and dried at 90° in vacuum overnight, obtaining 2-p-chlorophenyl-2,3,5,6,7,8,9,10-octahydrocyclohepta[b]pyrazolo[3,4-d]pyridin-3-one hydrochloride, m.p. 272°-275°.

後処理

  1. temperatureis refluxed overnight under nitrogen atmosphere
  2. customThe solid precipitate is collected
  3. customtriturated with ether
  4. dissolutiondissolved in hot ethanol
  5. concentrationconcentrated to a smaller volume
  6. additiondiluted with ether
  7. customto precipitate a yellow solid, which
  8. customis collected
  9. washwashed with ether
  10. customdried at 90° in vacuum overnight

出典と根拠

ORDレコード
ord-a5fc0a92551144c7ab2fccb852bbbce0
出典データセット
uspto-grants-1988_04
特許番号
US04740512

反応ノート

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