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Carbon Dioxide → N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)-N'-methyl-3,4,5,6-tetrahydrophthalamide

HRID 742416
ノート
印刷プレビュー

反応式

HRID 742416 の反応式
Cl.[CH3:2][NH2:3].C(=O)([O-])[O-].[K+].[K+].C(=O)=O.[F:13][C:14]1[CH:19]=[C:18]([Cl:20])[C:17]([O:21][CH:22]2[CH2:26][CH2:25][CH2:24][CH2:23]2)=[CH:16][C:15]=1[N:27]1[C:31](=[O:32])[C:30]2[CH2:33][CH2:34][CH2:35][CH2:36][C:29]=2[C:28]1=[O:37]>C(#N)C>[F:13][C:14]1[CH:19]=[C:18]([Cl:20])[C:17]([O:21][CH:22]2[CH2:26][CH2:25][CH2:24][CH2:23]2)=[CH:16][C:15]=1[NH:27][C:28](=[O:37])[C:29]1[CH2:36][CH2:35][CH2:34][CH2:33][C:30]=1[C:31]([NH:3][CH3:2])=[O:32]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 280Carbon DioxideHCID 11430Potassium CarbonateHCID 6364545Methylamine hydrochlorideHCID 15279390N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)-3,4,5,6-tetrahydrophthalimide

生成物 1

HCID 19425267N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)-N'-methyl-3,4,5,6-tetrahydrophthalamide収率 74.9%

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒

実験手順

Methylamine hydrochloride (1.70 g, 24.8 mmol) and potassium carbonate (1.70 g, 12.3 mmol), and acetonitrile (5 ml) as a solvent were placed into a round bottom flask (100 cc), followed by stirring at room temperature. After confirming the generation of carbon dioxide gas, N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)-3,4,5,6-tetrahydrophthalimide (5.88 g, 16.2 mmol) was added thereto, followed by stirring at room temperature for 4 hours. After completion of the reaction, the solvent was distilled off under reduced pressure, and the precipitated crystals were isolated by filtration. The crystals were washed with hexane and dried to obtain N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)-N'-methyl-3,4,5,6-tetrahydrophthalamide as white crystals (4.79 g, 74.9% yield).

後処理

  1. additionwas added
  2. stirringby stirring at room temperature for 4 hours
  3. customAfter completion of the reaction
  4. distillationthe solvent was distilled off under reduced pressure
  5. customthe precipitated crystals were isolated by filtration
  6. washThe crystals were washed with hexane
  7. customdried

出典と根拠

ORDレコード
ord-35317fcec12c477494b8d1a0edbda808
出典データセット
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05554581

反応ノート

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