(4-Chlorophenyl)hydrazine → HCID 178479604, 화합물

HRID 1905683노트

반응식

HRID 1905683 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 178479604HCID 178479604, 화합물

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-e8e735b8ca0a4d7fa4efbdf89c4b1ace
출처 데이터셋
uspto-grants-1987_03
특허 번호
US04647566

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