Triethylamine → 8-Fluoro-11(1-ethoxycarbonyl-4-piperidylidene)-6,11-dihydro-5H-benzo[5,6]cyclohepta[1,2-b]pyridine

HRID 542756ノート

反応式

HRID 542756 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)[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:23]=1.C(N(CC)CC)C.[CH2:31]([O:33][C:34](Cl)=[O:35])[CH3:32]>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:3]=[CH:4][C:5]2[C:15](=[C:16]3[CH2:17][CH2:18][N:19]([C:34]([O:33][CH2:31][CH3:32])=[O:35])[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:23]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 13920595HCID 13920595、化合物

生成物 1

HCID 139205968-Fluoro-11(1-ethoxycarbonyl-4-piperidylidene)-6,11-dihydro-5H-benzo[5,6]cyclohepta[1,2-b]pyridine収率 81.1%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a stirred solution of 8-fluoro-11-(1-methyl-4-piperidylidene)-6,11-dihydro-5H-benzo[5,6]cyclohepta[1,2-b]pyridine (10.5 g, 34 mmol) and triethylamine (5.2 g, 52 mmol) in dry toluene (120 mL) at 80° C. under an argon atmosphere, was added ethylchloroformate (18.5 g, 170 mmol) via a syringe. The reaction mixture was allowed to stir at this temperature for 30 minutes and at room temperature for one hour. The reaction mixture was then filtered and solvent was removed. The residue was triturated with pentane to give 10.1 grams (yield=81%) of the title compound, m.p.=116°-118° C.

後処理

  1. filtrationThe reaction mixture was then filtered
  2. customsolvent was removed
  3. customThe residue was triturated with pentane

出典と根拠

ORDレコード
ord-76754af54ece4b7a862d53b27e26178c
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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