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Dimethylformamide → N1-Cyclopropyl-5-({2-[(cyclopropylcarbonyl)amino]-4-pyridyl}oxy)-1H-1-indolecarboxamide

HRID 853350
ノート
印刷プレビュー

反応式

HRID 853350 の反応式
[CH:1]1([NH:4][C:5]([N:7]2[C:15]3[C:10](=[CH:11][C:12]([O:16][C:17]4[CH:22]=[CH:21][N:20]=[C:19]([N:23](C(C5CC5)=O)[C:24]([CH:26]5[CH2:28][CH2:27]5)=[O:25])[CH:18]=4)=[CH:13][CH:14]=3)[CH:9]=[CH:8]2)=[O:6])[CH2:3][CH2:2]1.[Cl-].[NH4+].CN(C)C=O>C(OCC)(=O)C.O.C(O)C>[CH:1]1([NH:4][C:5]([N:7]2[C:15]3[C:10](=[CH:11][C:12]([O:16][C:17]4[CH:22]=[CH:21][N:20]=[C:19]([NH:23][C:24]([CH:26]5[CH2:28][CH2:27]5)=[O:25])[CH:18]=4)=[CH:13][CH:14]=3)[CH:9]=[CH:8]2)=[O:6])[CH2:3][CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 6228DimethylformamideHCID 25517Ammonium ChlorideHCID 22936650N1-Cyclopropyl-5-({2-[di(cyclopropylcarbonyl)amino]-4-pyridyl}oxy)-1H-1-indolecarboxamide

生成物 1

HCID 58930818N1-Cyclopropyl-5-({2-[(cyclopropylcarbonyl)amino]-4-pyridyl}oxy)-1H-1-indolecarboxamide収率 41%

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒
HCID 962Water溶媒2 回
HCID 8857Ethyl Acetate溶媒

実験手順

N1-Cyclopropyl-5-({2-[di(cyclopropylcarbonyl)amino]-4-pyridyl}oxy)-1H-1-indolecarboxamide (190 mg), ammoniumchloride (660 mg), dimethylformamide (5 ml), water (5 ml) and ethanol (5 ml) were stirred at 100° C. for 1 hour. Water and ethyl acetate were added for extraction, and the extract was washed 6 times with water. After drying over magnesium sulfate, the drying agent was filtered off and the solvent was distilled off under reduced pressure. Ethyl acetate was added to the residue and the precipitated solid was filtered out to obtain 66 mg of a white powder.

後処理

  1. washthe extract was washed 6 times with water
  2. dry with materialAfter drying over magnesium sulfate
  3. filtrationthe drying agent was filtered off
  4. distillationthe solvent was distilled off under reduced pressure
  5. additionEthyl acetate was added to the residue
  6. filtrationthe precipitated solid was filtered out

出典と根拠

ORDレコード
ord-8422deadada64146851b17aaa1fce1ad
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07253286B2

反応ノート

読み込み中…

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