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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Methyl iodide → HCID 19434922、化合物

HRID 1736147
ノート
印刷プレビュー

反応式

HRID 1736147 の反応式
[NH2:1][C:2]1[C:7]2[C:8](=[O:27])[CH:9]=[C:10]([C:12]3[CH:17]=[CH:16][C:15]([NH:18][C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])=[C:14]([F:26])[CH:13]=3)[O:11][C:6]=2[C:5]([F:28])=[CH:4][C:3]=1[F:29].[H-].[Na+].I[CH3:33].[Cl-].[NH4+]>CN(C)C=O>[NH2:1][C:2]1[C:7]2[C:8](=[O:27])[CH:9]=[C:10]([C:12]3[CH:17]=[CH:16][C:15]([N:18]([C:19]([O:21][C:22]([CH3:25])([CH3:23])[CH3:24])=[O:20])[CH3:33])=[C:14]([F:26])[CH:13]=3)[O:11][C:6]=2[C:5]([F:28])=[CH:4][C:3]=1[F:29]
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 6328Methyl iodideHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 19434972HCID 19434972、化合物

生成物 1

HCID 19434922HCID 19434922、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1.99 g (4.73 mmol) of Compound 51 obtained in Example 51 was dissolved in 80 ml of dimethylformamide under argon atmosphere, 212 mg. of sodium hydride (60% oil disperison) and 0.60 ml of iodomethane were added and the mixture was stirred at room temperature for 1 hour. An aqueous saturated solution of ammonium chloride was added to the reaction solution, the precipitated crystals were collected by filtration and dissolved in ethanol, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (chloroform) to give 2.09 g of 5-amino-2-[4-[N-(tert-butoxycarbonyl)-N-methylamino]-3-fluorophenyl]-6,8-difluoro-4H-1-benzopyran-4-one.

後処理

  1. filtrationthe precipitated crystals were collected by filtration
  2. dissolutiondissolved in ethanol
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (chloroform)

出典と根拠

ORDレコード
ord-9f94627440b14c3e95b2c210e4f379c5
出典データセット
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05539112

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート