Potassium Hydroxide → 8-fluoro-11-(4-piperidylidene)-6,11-dihydro-5H-benzo[5,6]cyclohepta[1,2-b]pyridine

HRID 542757ノート

反応式

HRID 542757 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[C:15](=[C:16]3[CH2:21][CH2:20][N:19](C(OCC)=O)[CH2:18][CH2:17]3)[C:10]3=[N:11][CH:12]=[CH:13][CH:14]=[C:9]3[CH2:8][CH2:7][C:6]=2[CH:27]=1.[OH-].[K+]>C(O)C.O.[Cl-].[Na+].O>[F:1][C:2]1[CH:3]=[CH:4][C:5]2[C:15](=[C:16]3[CH2:17][CH2:18][NH:19][CH2:20][CH2:21]3)[C:10]3=[N:11][CH:12]=[CH:13][CH:14]=[C:9]3[CH2:8][CH2:7][C:6]=2[CH:27]=1

参加物

5

反応物 2

HCID 14797Potassium HydroxideHCID 139205968-Fluoro-11(1-ethoxycarbonyl-4-piperidylidene)-6,11-dihydro-5H-benzo[5,6]cyclohepta[1,2-b]pyridine

生成物 1

HCID 139205978-fluoro-11-(4-piperidylidene)-6,11-dihydro-5H-benzo[5,6]cyclohepta[1,2-b]pyridine収率 95.7%

試薬・触媒・溶媒 2

HCID 19096565Water ethanol溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

8-Fluoro-11-(1-ethoxycarbonyl-4-piperidylidene)-6,11-dihydro-5H-benzo[5,6]cyclohepta[1,2-b]pyridine (3.6 g, 9.8 mmol.) was refluxed with KOH (4.5 g) in 50 mL of ethanol/water (1:1) for 66 hours under an argon atmosphere. The reaction mixture was poured into a brine solution and extracted twice with ethyl acetate. The extracts were combined and then dried over Na2SO4 and filtered. Solvent was removed to give 2.76 grams (yield=95%) of the title compound, m.p.=133.5°-134.5° C.

後処理

  1. extractionextracted twice with ethyl acetate
  2. dry with materialdried over Na2SO4
  3. filtrationfiltered
  4. customSolvent was removed

出典と根拠

ORDレコード
ord-304ceaeaba1f4aec9ead2888124616f5
出典データセット
uspto-grants-1987_04
特許番号
US04659716

反応ノート

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