Maleic Acid → 4-[2-[4-(1H-indole-3-yl)-1-piperidinyl]ethyl]-2(1H)-quinolinone maleate

HRID 2209970ノート

反応式

HRID 2209970 の反応式
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([CH:10]2[CH2:15][CH2:14][N:13]([CH2:16][CH2:17][C:18]3[C:27]4[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=4)[NH:21][C:20](=[O:28])[CH:19]=3)[CH2:12][CH2:11]2)=[CH:2]1.[C:29]([OH:36])(=[O:35])/[CH:30]=[CH:31]\[C:32]([OH:34])=[O:33]>CO.O1CCCC1>[C:29]([OH:36])(=[O:35])/[CH:30]=[CH:31]\[C:32]([OH:34])=[O:33].[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([CH:10]2[CH2:15][CH2:14][N:13]([CH2:16][CH2:17][C:18]3[C:27]4[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=4)[NH:21][C:20](=[O:28])[CH:19]=3)[CH2:12][CH2:11]2)=[CH:2]1

参加物

5

反応物 2

HCID 444266Maleic AcidHCID 3073949Swr 00151

生成物 1

HCID 677852834-[2-[4-(1H-indole-3-yl)-1-piperidinyl]ethyl]-2(1H)-quinolinone maleate収率 61.4%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 4-[2-[4-(1H-indole-3-yl)-1-piperidinyl]ethyl]-2(1H)-quinolinone (III-2) (500 mg, 1.35 mmol) in methanol (15 ml) and tetrahydrofuran (25 ml) was refluxed until solids were dissolved. Under the same conditions, maleic acid (172.9 mg, 1.49 mmol) in methanol (10 ml) was added thereto and then the solvent was distilled off from the reaction mixture. The residue was crystallized with acetone and then recrystallized from acetone-methanol to give the desired product (III'-2-b) (404 mg) as pale yellow crystals (138°-141 ° C., yield 61.4%)

後処理

  1. temperaturewas refluxed until solids
  2. dissolutionwere dissolved
  3. distillationthe solvent was distilled off from the reaction mixture
  4. customThe residue was crystallized with acetone
  5. customrecrystallized from acetone-methanol

出典と根拠

ORDレコード
ord-e6cdfea81df74dbd95e854fb494ab13f
出典データセット
uspto-grants-1995_10
特許番号
US05457099

反応ノート

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